Quick Details Classification: Chemical Auxiliary Agent CAS No.: 12079-65-1 Other Names: cymantren MF: C8H5MnO3 EINECS No.: 235-142-4 Purity: 98.0%min
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inquiryCyclopentadienylmanganese Tricarbonyl CAS 12079-65-1 tricarbonyl(η-cyclopentadienyl)manganese CAS no 12079-65-1 Manganese, tricarbonyl(h5-2,4-cyclopentadien-1-yl)- Cyclopentadienylmanganese Tricarbonyl High quality Best price In stock fact
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inquiryAppearance:yellow powder Storage:under inert gas (nitrogen or Argon) at 2-8°C Package:25kg/drum Application:chemicals Transportation:Express/Sea/Air Port:Shanghai
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inquiryProduct Name: CYCLOPENTADIENYLMANGANESE TRICARBONYL Synonyms: CYCLOPENTADIENYLMANGANESE TRICARBONYL;CYCLOPENTADIENYLTRICARBONYLMANGANESE;tricarbonyl(eta-cyclopentadienyl)manganese;Cyclopentadienyl marganese tricarbonyl;Cyclopentadienylmanganese
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inquiryConditions | Yield |
---|---|
in sealed tube at 200°C; | A 96% B 96% |
triethyl phosphite
A
cymantrene
D
[Mn(C5H5)(CO)2(P(OC2H5)3)]
E
(C5H5)(CO)[P(OCH2CH3)3]MnCCHC6H5
Conditions | Yield |
---|---|
In hexane at 20°C under Ar, 1 h; evapn., chromy. (Al2O3, hexane/ether, then ether), recrystn. (hexane/ether)., elem. anal.; | A n/a B 96% C n/a D n/a E <1 |
dimethylsulfide borane complex
A
cymantrene
B
[(η5-cyclopentadienyl)Mn(CO)2SMe2]
C
triphenylphosphine borane
Conditions | Yield |
---|---|
In toluene Inert atmosphere; Schlenk technique; | A n/a B n/a C 95% |
triisopropyl phosphite
A
cymantrene
Conditions | Yield |
---|---|
In hexane under Ar; addn. of P(O-i-Pr)3 hexane soln. to hexane soln. of complex, mixed 3h at 20°C; evapn., residue is dissolved in 1:1 hexane-diethyl ether mixt., chromd. (Al2O3), mixt. of CpMn(CO)3 and Cp(CO)2MnCCPhH, yellow band eluted with 1:1 hexane-methyl acetate, evapn. of solvent, oily residue treated with hexane/benzene, elem. anal.; | A n/a B 92% |
cyclopentadienyl manganese tricarbonyl(1+)
cymantrene
Conditions | Yield |
---|---|
In dichloromethane Electrolysis; controlled potential electrolysis at 0.5 V, CH2Cl2/0.05 M N(C4H9)4B(C6F5)4; electrochemical IR-spectra; | 90% |
triiron dodecarbonyl
1-butanethiol
triethylamine
A
cymantrene
Conditions | Yield |
---|---|
In tetrahydrofuran N2-atmosphere; stirring (room temp., 40 min), Mn-compd. addn., stirring (-90 to -70°C, 3 h); evapn. (vac., -50 to -40°C), chromy. (alumina, -25°C, petroleum ether, petroleum ether / CH2Cl2 = 20 : 1, petroleum ether / CH2Cl2/ Et2O = 10 : 1 : 1), evapn. (vac.), recrystn. (petroleum ether / CH2Cl 2, -80°C); elem. anal.; | A 3% B 85% C 6% D 4% |
Conditions | Yield |
---|---|
In benzene Ar-atmosphere, dry solvent; Fe-compd. addn. to soln. of Mn,Pd-complex, stirring (3 h, 20°C), soln. filtration through Al2O3, vacuum evapn.; oily residue dissoln. in hexane-benzene, chromy. (Al2O3/hexane-benzene),eluate fractions evapn.; elem. anal.; | A n/a B 71% C 5% D 9% |
triiron dodecarbonyl
Benzeneselenol
A
cymantrene
B
C5H5Mn(CO)2Fe(CO)3CC6H5SeC6H5
C
(μ-PhSe)2Fe2(CO)6
Conditions | Yield |
---|---|
With N(CH2CH3)3 In tetrahydrofuran (N2); addn. of selenium compd. and amine to a soln. of iron carbonyl in THF, stirring at room temp. for 10 min, cooling to -100°C, pouring to manganese complex, warming to -80°C, stirring for 7 h at -80to -50°C; evapn. at -50 to -40°C, column chromy (Al2O3, petroleum ether, petroleum ether/CH2Cl2 20:1, petroleum ether/CH2Cl2/Et2O 10:1:1), evapn., recrystn. (petroleum ether/CH2Cl2, -80°C); elem. anal.; | A 5% B 66% C 24% |
A
cymantrene
Conditions | Yield |
---|---|
With Pt(P(C6H5)3)4 In benzene a soln. of Mn-compd. (0.22 mmol) and Pt-compd. (0.20 mmol) in benzene was stirred under Ar at 20°C for 4 h;; evapn.; the residue was dissolved in hexane-benzene mixt. (2:1) and chromd. (alumina, hexane-benzene); removal of the solvent; residue was dissolved in ether; crystn. after cooling at -20°C;; | A n/a B 65% |
dichloromethane
A
cymantrene
Conditions | Yield |
---|---|
In toluene (N2, Schlenk technique); addn. of molybdenum compd. to THF soln. of manganese compd., dissolving in toluene, stirring at room temp. for 15 min; evapn., extn. (CH2Cl2/petroleum ether (1:7)), chromy. (alumina, CH2Cl2/petroleum ether 1:7, then 1:1) at 253 K, evapn., elem. anal.; | A n/a B 65% |
A
cymantrene
Conditions | Yield |
---|---|
In pentane Ar atmosphere; stirring (20°C, 24 h); TLC (petroleum); | A n/a B 32% C 64% |
triiron dodecarbonyl
p-Selenocresol
A
cymantrene
B
(μ-p-MeC6H4Se)2Fe2(CO)6
C
C5H5Mn(CO)2Fe(CO)3CC6H5SeC6H4CH3
Conditions | Yield |
---|---|
With N(CH2CH3)3 In tetrahydrofuran (N2); addn. of selenium compd. and amine to a soln. of iron carbonyl in THF, stirring at room temp. for 10 min, cooling to -100°C, pouring to manganese complex, warming to -80°C, stirring for 7-8 h at -80 to -45°C; evapn. at -50 to -40°C, column chromy (Al2O3, petroleum ether, petroleum ether/CH2Cl2 20:1, petroleum ether/CH2Cl2/Et2O 10:1:1), evapn., recrystn. (petroleum ether/CH2Cl2, -80°C); elem. anal.; | A 6% B 25% C 63% |
tetramethylammonium hydridoirontetracarbonyl
A
cymantrene
Conditions | Yield |
---|---|
In tetrahydrofuran (N2); addn. of the Mn complex at -90°C to the Fe compd. in THF with vigorous stirring, further stirring (-90 to -45°C, 4 h); evapn. to dryness (high vacuum, -45 to -40°C), chromy. (neutral alumina; light petroleum, then light petroleum/CH2Cl2; -25°C), collection, solvent removal (vac.), recrystn. (light petr. or light petr./CH2Cl2 at -80°C); elem. anal.; | A 25% B 63% |
A
cymantrene
Conditions | Yield |
---|---|
In dichloromethane Ar atmosphere; stirring (20°C, 6 h); evapn. (vac.), extn. (CHCl3), chromy. (SiO2, petroleum ether, petroleumether/CHCl3 50:1, 5:1 and 2:1); elem anal.; | A n/a B 5% C 4.5% D 60% E 10% |
Conditions | Yield |
---|---|
In benzene under Ar; stirred at 70°C for 30 min; filtration (0.5 cm Al2O3), concn. in vac., chromy. (Al2O3, hexane-benzene), elem. anal.; | A n/a B 53% C 28% D >1 |
Conditions | Yield |
---|---|
In tetrahydrofuran (N2); bubbling CO gas through a soln. of the Mn-Fe complex in THF at -40to -10°C for 4 h; removal of solvent (vac.), chromy. (neutral alumina; light petroleum, then light petroleum/CH2Cl2), collection, removal of solvents (vac.), recrystn. (light petroleum or light petroleum/CH2Cl2; -80°C); elem. anal.; | A 31% B 46% |
A
cymantrene
Conditions | Yield |
---|---|
In tetrahydrofuran (N2); addn. of the Mn complex to the Fe complex salt in THF with stirring at -90°C, further stirring (-90 to -80°C, 1 h, -60°C, 3 h); solvent removal (vac., -40°C), chromy. (-25°C, neutral alumina; light petroleum/CH2Cl2, then light petroleum/CH2Cl2/Et2O); | A 26% B 44% |
silver(I) hexafluorophosphate
C5H5(CO)2MnSC6H4NO2
A
cymantrene
B
{C5H5(CO)2Mn}2SC6H4NO2(1+)*PF6(1-)*0.5CH2Cl2 = {C5H5(CO)2Mn}2SC6H4NO2PF6*0.5CH2Cl2
Conditions | Yield |
---|---|
In toluene carried out with exclusion of air and moisture; 1 equiv of AgPF6 added to a stirred soln. of the Pd complex; mixt. stirred for further 20 min. at room temp.; volume reduced in vac., pentane added, filtered through silanized silica gel, elution with CH2Cl2, crystn. from CH2Cl2-Et2O (1:1) at -30°C; elem. anal.; | A n/a B 42% |
A
cymantrene
Conditions | Yield |
---|---|
With hydrogenchloride; phenyllithium In diethyl ether byproducts: LiCl; Ar atmosphere; addn. of PhLi in ether to soln. of Mn-complex, stirring (-60°C, 30 min, at -20°C fo 30 min), acidification (HCl inether); sepn. of LiCl, filtration), evapn. (vac.), chrpmy. (5°C, ether/CH2Cl2 (1:4), ether); | A n/a B 40% |
A
cymantrene
Conditions | Yield |
---|---|
In tetrahydrofuran (N2); addn. of the Mn complex to the Fe complex salt in THF with stirring at -90°C, further stirring (-90 to -80°C, 1 h), warming to -50°C over 3 h; evapn. to dryness (high vac., -40°C), chromy. (-25°C, neutral alumina; light petroleum/CH2Cl2, then light petroleum/CH2Cl2/Et2O); elem. anal.; | A 23% B 39% C 19% |
A
cymantrene
Conditions | Yield |
---|---|
With phenyllithium In diethyl ether byproducts: LiCl; addn. of 1 N soln. of C6H5Li in ether (4.06 mmol) to soln. of (C5H5)(OC)2Mn(CHCCH(CH3)OH) (4.06 mmol) in ether, stirring mixt. for 0.5 h at-60°C, 0.5 h at -20°C, acidifying with 1 N HCl in ether (dry solvents, Ar-atmosphere); filtering to remove LiCl, evapg. solvent in vac., chromy. of residue on SiO2-column (5°C), eluation with ether (elem. anal.); | A n/a B 35% |
Conditions | Yield |
---|---|
In tetrahydrofuran; acetone byproducts: Me3SiOH; Irradiation (UV/VIS); under Ar, soln. of Mn-complex was stirred for 4-5 h at -15 °C during irradn. with Hg-lamp., sulfinylimide was used in slight excess, soln. was warmed up to room temp. after 30 min, stirring for 2-3 h; soln. was evapd. in vac., subl., residue was dissolved in wet acetone, mixt. was stood for several days at room temp., elem. anal.; HNSO-complexwas not isolated, detected by spectr. methods; | 99% |
Conditions | Yield |
---|---|
In tetrahydrofuran; acetone byproducts: PhNH2; Irradiation (UV/VIS); under Ar, soln. of Mn-complex was stirred for 4-5 h at -15 °C during irradn. with Hg-lamp., sulfinylimide was used in slight excess, soln. was warmed up to room temp. after 30 min, stirring for 2-3 h; soln. was evapd. in vac., subl., residue was dissolved in wet acetone, mixt. was stood for several days at room temp., elem. anal.; | 99% |
cymantrene
Conditions | Yield |
---|---|
With CH3COCl; AlCl3 In dichloromethane byproducts: HCl; (Ar), to CH3COCl in CH2Cl2 added AlCl3 for 10 min, Mn-complex in CH2Cl2 added dropwise for 3 h; hydrolysed, HCl added, extracted, washed with H2O, dried over Na2SO4, filtered, solvent removed in vac.; | 96% |
Conditions | Yield |
---|---|
palladium(II) oxide In toluene byproducts: CO; (Ar); soln. of Mn complex and PdO was heated to reflux and the isonitrilederiv. was added, refluxing was continued for 6 h, react. was monitored by TLC; chromy. (Kieselgel, CH2Cl2/hexane); recrystn. from CH2Cl2/hexane; elem. anal.; | 95% |
cymantrene
N,N-dimethyl-formamide
Conditions | Yield |
---|---|
Stage #1: cymantrene With n-butyllithium In tetrahydrofuran; hexane at -78℃; Inert atmosphere; Stage #2: N,N-dimethyl-formamide In tetrahydrofuran; hexane at -78 - 20℃; for 2h; | 94.5% |
With n-butyllithium; ammonium chloride In tetrahydrofuran; Petroleum ether byproducts: (CH3)2NH; Ar; soln. of (OC)3MnC5H4Li, prepd. at -50°C from soln. of (OC)3MnC5H5 and soln. of n-butyl lithium in THF, cooled to -70°C, addedin 2-5 min to DMF; mixt. stirred (1-1.5 h, -10 - -5°C); satd. soln. of NH4Cl in H2O added; aq. layer washed (ether); org. extract dried (MgSO4); solvent distilled off; residue chromd. (SiO2, 1/2 petroleum ether-benzene); | 75% |
With n-C4H9Li; NH4Cl In N,N-dimethyl-formamide (Ar); treatment soln. of cymantrene/THF with n-BuLi/C6H14 at -50°C for 15 min, cooling, transferring into Schlenk tube with DMF; stirringat 0°C for 90 min, addn. of soln. of NH4Cl; Bull. SSSR Acad. of Sci., Div. of Chemistry 29 (1990)2387; | 72% |
cymantrene
Conditions | Yield |
---|---|
With THF In tetrahydrofuran byproducts: CO; Irradiation (UV/VIS); irradn. until end of gas-evolution, 24 h stirred at 25°C, addn. of further C5H5Mn(CO)2(THF), stirred 24 h at 25°C.; recrystn. from THF-hexane; elem. anal.; | 94% |
cymantrene
trimethyl(methylene)phosphorane
Conditions | Yield |
---|---|
In pentane stirred at 25°C for 20 min; cooling at 0°C, ppt. washed with ice-cold pentane, dried at 25°C, elem. anal.; | 93% |
Methyltrichlorosilane
cymantrene
tris(η5-cyclopentadienyl(tricarbonyl)manganese)methylsilane
Conditions | Yield |
---|---|
With s-BuLi In tetrahydrofuran; cyclohexane To a soln. of Fe-compd. in THF a soln. of s-BuLi is added at -78°C, mixt. is stirred for 20 min. CH3SiCl3 is added dropwise via a syringe at -78°C, mixt. is allowed to warm to 20°C (N2).; Solvent is removed in vac., residue is chromd on alumina III, elem. anal.; | 93% |
Conditions | Yield |
---|---|
In neat (no solvent) byproducts: HBr; under N2; cymantrene dissolved in neat BBr3; refluxed for 44 h; HBr condensed into cold trap (liq. N2); react. mixt. cooled to room temp.; filtered; filtrate evapd. slowly in vac.; detd. by X-ray powder diffraction; | 93% |
cymantrene
Conditions | Yield |
---|---|
With n-butyl lithium; copper(II) chloride In diethyl ether; hexane ether soln. of CpMn(CO)3 was treated with hexane soln. of n-BuLi at -70°C in anaerobic conditions, stirred for 1 h at this temp., anhyd. CuCl2 was added, suspn. was stirred for 3 h at -60°C and brought to room temp. within 5 h; hydrolyzed (H2O), ether phase dried, evapd., residue was sublimed at 110°C under high vac.; elem. anal.; | 92% |
8-bromoquinoline
cymantrene
tricarbonyl[η5-(8-quinolyl)cyclopentadienyl]manganese(I)
Conditions | Yield |
---|---|
With n-butyllithium; ZnCl2; bis(triphenylphosphine)palladium(0) In tetrahydrofuran byproducts: LiCl; 1.) n-BuLi in hexane (-78°C), stirred for 1 h; 2.) ZnCl2 in THF, stirred for 1 h; 3.) Pd(PPh3)2, 8-bromoquinoline were added dropwise, the soln. was allowed to warm to room temp., stirred for 5 d (Ar, protection against light); aq. NaOH was added, stirred for 1.5 h, the organic layer was sepd., extd. with THF, dried (MgSO4), filtered, evapd., chromy. on Al2O3/5% H2O with toluene, elem. anal.; | 92% |
cymantrene
propionyl chloride
(Propionylcyclopentadienyl)tricarbonylmanganese
Conditions | Yield |
---|---|
aluminium trichloride In carbon disulfide (Ar); Schlenk tube; AlCl3 was added to soln. of cymantrene and propionylchloride in CS2; after 1.5 h CS2 was removed in vac.; water was added at 0°C; extd. (Et2O); dried (MgSO4); soln. concd.; pentane added; recrystd. (Et2O/pentane); elem. anal.; | 92% |
With AlCl3 In carbon disulfide (Ar); addn. of AlCl3 to a soln. of manganese complex in CS2, addn. of a soln. of propionyl chloride in CS2, stirring for 1.5 h; evapn., addn. of water at 0°C, extn. with Et2O, drying (MgSO4), concn., addn. of pentane, recrystn. (ether/ pentane); elem. anal.; | 92% |
With aluminum (III) chloride In dichloromethane at 20℃; for 4h; Schlenk technique; | 71% |
cymantrene
buta-1,3-diene
Conditions | Yield |
---|---|
In diethyl ether; water Irradiation (UV/VIS); N2 atmosphere; addn. of org. comp. and aq. soln. of HPF6 to soln. of Mn-compd. in Et2O, purging with N2, stirring, irradiation without stirring (15-25°C, 15-30 min, 365 nm); 22% conversion; filtn., washing (ether), precipitaion from acetone/ether (0°C); elem. anal.; | 91% |
n-butyllithium
cymantrene
tungsten hexacarbonyl
N,N,N,N,-tetramethylethylenediamine
trifluoroacetic anhydride
Conditions | Yield |
---|---|
In tetrahydrofuran; diethyl ether; hexane treating 31 mmol (Mn(CO)3(C5H5)) in THF/ ether at -80°C with 32.0 mmol LiC4H9 in hexane; stirring for 1 h; addn. of 31.3 mmol (W(CO)6); stirring at -10°C for 1 h; cooling to -80°C; treating with (CF3CO)2O in THF; addn. of ligand;; warming to room temperature; evaporation under reduced pressure; extraction with dichloromethane; chromy. (CH2Cl2); concn. in vac.; diln. with petroleum; cooling to -80°C; pptn.; decantation; washing with petroleum; drying in vac.; elem. anal.;; | 91% |
oxirane
cymantrene
p-toluenesulfonyl chloride
(η(5)-C5H4CH2CH2OSO2C6H4CH3)Mn(CO)3
Conditions | Yield |
---|---|
With n-butyllithium In tetrahydrofuran; pentane byproducts: LiCl; N2-atmosphere; addn. of equimolar amt. of BuLi (in pentane) to Mn-complex soln. (in THF) at -78°C, addn. of slight excess of ethylene oxide (after 3 h, -78°C), warming to 0°C (after 2 h), addn. of equimolar amt. of tosyl chloride; solvent removal (after 30 min, 25°C, vac.), extn. into CH2Cl2, filtration off of LiCl (Celite), evapn., chromy. (SiO2, CH2Cl2); elem. anal.; | 91% |
Conditions | Yield |
---|---|
Stage #1: cymantrene With n-butyllithium In tetrahydrofuran; hexane at -80℃; for 1.5h; Schlenk technique; Inert atmosphere; Stage #2: oxirane In tetrahydrofuran; hexane at -80 - 25℃; Schlenk technique; Inert atmosphere; Stage #3: With water In tetrahydrofuran; hexane at 25℃; Schlenk technique; Inert atmosphere; | 91% |
Conditions | Yield |
---|---|
In further solvent(s) Irradiation (UV/VIS); cymantrene soln. in subcritical and supercritical ethylene (-40 - 50°C, 35-2600 bar), photolysis (10 h); not isolated; | 90% |
tetrahydrofuran
cymantrene
tetracarbonylbis(η5-cyclopentadienyl)-μ4-diarsenic-dimolybdenum (Mo-Mo)
A
tetracarbonylbis(η5-cyclopentadienyl)μ4-diarsenic-bis{dicarbonyl(η5-cyclopentadienyl)manganese}dimolybdenum (Mo-Mo)
B
carbon monoxide
Conditions | Yield |
---|---|
In tetrahydrofuran Irradiation (UV/VIS); 4.90 mmol (C5H5)Mn(CO)3 in THF photolyzed for 90 min; soln. concd. and added to 4.28 mmol (C5H5)2Mo2(CO)4As2; soln. stirred for 6 h at room temp.; solvent concd.; chromy. (silica gel) with hexane yields (C5H5)Mn(CO)3, then with toluene/ether (1:1) (CpMo(CO)2)2(CpMn(CO)2As)2 which is crystd. from CH2Cl2/hexane at -18°C; elem. anal.; | A 90% B n/a |
cymantrene
(η5-C5H4(COPh))Re(CO)3
Conditions | Yield |
---|---|
With n-butyllithium; N,N,N,N,-tetramethylethylenediamine In tetrahydrofuran; hexane cymantrenyllithium prepd. above -78°C from cymantrene, TMEDA, and n-BuLi; after 45 min, the Re complex is added; mixt. warmed to room temp. for 20 h; hydrolyzed; washed with distilled water; solvent removed under high vac.; chromy on silica with dichloromethane/hexane eluent; recrystd. from ethanol/water; elem. anal.; | 90% |
cymantrene
methyl isocyanate
Conditions | Yield |
---|---|
In tetrahydrofuran byproducts: CO; Irradiation (UV/VIS); N2-atmosphere; equimolar amts.or excess MeNC, 100-W Hg lamp (18 h); evapn., chromy. (Al2O3), evapn., crystn. (-78°C, petroleum ether); elem. anal.; yield related to equimolar amts. of educts; | 90% |
palladium(II) oxide In toluene byproducts: CO; (Ar); soln. of Mn complex and PdO was heated to reflux and the isonitrilederiv. was added, refluxing was continued for 24 h, react. was monitored by TLC; chromy. (Kieselgel, CH2Cl2/hexane); recrystn. from CH2Cl2/hexane; elem. anal.; | 5% |
cymantrene
[2,6-diphenylpyrylium](PF6)
trityl tetrafluoroborate
[(4-cyclopentadienyl-2,6-diphenylpyrylium)Mn(CO)3](BF4)
Conditions | Yield |
---|---|
With BuLi In tetrahydrofuran; diethyl ether; hexane N2-atmosphere; addn. of BuLi (hexane) to THF soln. of Mn-complex at -60°C, stirring for 1 h, addn. of pyrylium (THF:ether), warming to 0°C, addn. of aq. NH4Cl, extn. (ether), drying (MgSO4), chromy. (Al2O3, pentane), addn. of MeCN; addn. of Ph3CBF4, stirring for 30 min, addn. of ether, collection (filtration); elem. anal.; | 89% |
Conditions | Yield |
---|---|
With aluminum (III) chloride In dichloromethane at 20℃; for 5h; Friedel-Crafts Acylation; Schlenk technique; | 88% |
cymantrene
chloro-diphenylphosphine
tricarbonyl(η5-diphenylphosphinocyclopentadienyl)manganese
Conditions | Yield |
---|---|
With n-butyllithium In not given byproducts: LiCl; Complex was treated with n-BuLi at -70°C, PPh2Cl was added, the mixt. was kept at room temp. for 2 h;; aq. HCl was added with cooling, aq. NaOH was added to pH 8, extd. with ether or CH2Cl2, the organic layer was washed with water, evapd., crystd. from hexane or EtOH; elem. anal.;; | 87.4% |
cymantrene
Conditions | Yield |
---|---|
In tetrahydrofuran byproducts: CO; Irradiation (UV/VIS); irradiating a soln. of Mn(CO)3(C2H5) until the CO evolution beeing finished (ca 2 - 3 h), adding the Rh complex, stirring (ca 24 h, room temp.); concg., chromy. (Al2O3, benzene), recrystn. (pentane); | 87% |
In tetrahydrofuran byproducts: CO; Irradiation (UV/VIS); N2 atmosphere; photolysis of Mn-complex in THF (Hg-vapor lamp, 2-3 h), addn. of Rh-complex, stirring (room temp., 24 h); solvent removal, extraction (benzene), concn., chromy. (Al2O3, benzene/pentane 1:1), evapn. (vac.), crystn. (pentane, -78°C), collection (filtn.), washing (pentane), drying (vac.); elem. anal.; | 87% |
cymantrene
trisodium tris(3-sulfophenyl)phosphine
tris(natrium-m-sulfonatophenyl)phosphanoxid
Conditions | Yield |
---|---|
In tetrahydrofuran; water byproducts: CO; Irradiation (UV/VIS); (N2 or Ar); irradiation of soln. of Mn-complex in THF (high pressure Hg-lamp, 90 min, 15°C), addn. to org. compd. in H2O, stirring (16 h); phase sepn., washing org. phase (H2O), aq. phase (n-pentane), evapn. (vac.), chromy. (Sephadex), chromy. (Fractogel, H2O/EtOH); elem. anal.; | A 87% B 25% |
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