Conditions | Yield |
---|---|
In chloroform The Mo-compd. in CHCl3 is treated with (EtO)2PS2H and stirred 30 min.; Addn. of C6H6, centrifugation and decantation left the ammonium compd., which is further rinsed three times with C6H6, each time followed by centrifugation and decantation, and then dried.; | A 87% B n/a |
O,O-Diethyl hydrogen phosphorodithioate
A
bis(diethoxyphosphoryl)disulphide
B
ammonium O,O-diethyldithiophosphate
Conditions | Yield |
---|---|
In chloroform-d1 byproducts: acetic acid; To the Mo-compd. in CDCl3 is added (EtO)2PS2H, causing rapid darkening.; Pptn. of colorless crystals; (31)P-NMR and (1)H-NMR spectroscopy; |
tetrafluoroboric acid diethyl ether
ammonium O,O-diethyldithiophosphate
(η(5)-indenyl)Mo(CO)2(κ(2)-S2P(OEt))
Conditions | Yield |
---|---|
In dichloromethane Ar-atmosphere; stirring soln. of equimolar amts. of Mo-complex and HBF4 for 10 min, addn. of excess of (EtO)2PS2NH4, stirring for 10 h; filtration, evapn., extn. (hexane); elem. anal.; | 98% |
Conditions | Yield |
---|---|
In dichloromethane byproducts: NH4Cl; addn. of ZrCl4 in CH2Cl2 to a suspn. of the dithiophosphate in CH2Cl2 (1:4 molar ratio) under exclusion of moisture, refluxing (constant stirring, 6 h); filtration from pptd. NH4Cl4, removal of solvent (reduced pressure), washing (n-hexane), drying; elem. anal.; | 94% |
ammonium O,O-diethyldithiophosphate
trichlorodimethoxymolybdenum(V)
Conditions | Yield |
---|---|
In benzene byproducts: NH4Cl; exclusion of moisture, stirring equimolar amts. of trichloromethoxymolybdenum(V) and NH4S2P(OC2H5)2 for 2 h at room temp., change of colour from brown to green; filtering off pptd. NH4Cl, removing the solvent under reduced pressure at room temp., elem. anal.; | 93.3% |
ammonium O,O-diethyldithiophosphate
zinc(II) sulfate
bis(O,O-diethyldithiophosphato)zinc
Conditions | Yield |
---|---|
In water mixed; filtered; extd. (diethyl ether); dried (over MgSO4); evapd.; recrystd. (light petroleum); elem. anal.; | 90% |
ammonium O,O-diethyldithiophosphate
ethylphenyltin(IV) dichloride
(C2H5C6H5Sn(SSP(OC2H5)2)2)
Conditions | Yield |
---|---|
In hexane byproducts: NH4Cl; to a susp. of NH4SSP(OEt)2 in hexane a soln. of EtPhSnCl2 was added andthe reaction mixt. was allowed to stir for 2-3 h at room temp; NH4Cl formed during the reaction was filtered off, filtrate was concd. under vac., dissolving in anhydrous hexane, filtration through florisil under N2; elem. anal.; | 90% |
ammonium O,O-diethyldithiophosphate
dimethyltin dichloride
(CH3)2SnCl(SSP(OC2H5)2)
Conditions | Yield |
---|---|
In hexane byproducts: NH4Cl; to a susp. of NH4SSP(OEt)2 in hexane a soln. of Me2SnCl2 was added in 1:1 stoich. and the reaction mixt. was allowed to stir for 2-3 h at roomtemp; NH4Cl formed during the reaction was filtered off, filtrate was concd. under vac., elem. anal.; | 90% |
ammonium O,O-diethyldithiophosphate
methylphenyltin(IV) dichloride
(CH3C6H5Sn(SSP(OC2H5)2)2)
Conditions | Yield |
---|---|
In hexane byproducts: NH4Cl; to a susp. of NH4SSP(OEt)2 in hexane a soln. of MePhSnCl2 was added andthe reaction mixt. was allowed to stir for 2-3 h at room temp; NH4Cl formed during the reaction was filtered off, filtrate was concd. under vac., dissolving in anhydrous hexane, filtration through folrisil under N2; elem. anal.; | 89% |
ammonium O,O-diethyldithiophosphate
Conditions | Yield |
---|---|
In benzene byproducts: NH4Cl; moisture-free atmosphere; stirring with slight heating (45 - 50°C, 3 - 4 h); filtration, solvent removal (reduced pressure), recrystn. (benzene/petroleum ether = 1 : 1); elem. anal.; | 88% |
ammonium O,O-diethyldithiophosphate
MoI2(CO)3(MeCN)2
1,2-bis-(diphenylphosphino)ethane
Conditions | Yield |
---|---|
In dichloromethane byproducts: CO; MoI2(CO)3(NCMe)2 dissolved in CH2Cl2; solid NH4(S2P(OEt)2) added with stirring; after 30 min ppt. filtered off; to filtrate Ph2PCH2CH2PPh2 (ratio 1:1) added; soln. stirred for 30 min; concd.; hexane added; cooled down (-20°C) overnight; elem. anal.; | 87% |
ammonium O,O-diethyldithiophosphate
MoI2(CO)3(MeCN)2
1,2-bis-(diphenylphosphino)ethane
Conditions | Yield |
---|---|
In dichloromethane byproducts: CO; MoI2(CO)3(NCMe)2 dissolved in CH2Cl2; solid NH4(S2P(OEt)2) added with stirring; after 30 min ppt. filtered off; to filtrate Ph2PCH2CH2PPh2 added(ratio 2:1); soln. stirred for 30 min; concd.; hexane added; cooled down (-20°C) overnight; elem. anal.; | 87% |
ammonium O,O-diethyldithiophosphate
[Pd(PPh3)Cl]2(μ,η2-SCNMe2)2
[Pd(triphenylphosphine)(η1-CSNMe2)(η2-diethyldithiophosphate)]
Conditions | Yield |
---|---|
In CH2Cl2 under N2; Pd complex treated with NH4(S2P(OEt)2) in CH2Cl2 at ambient temp.; | 87% |
ammonium O,O-diethyldithiophosphate
Conditions | Yield |
---|---|
In dichloromethane Addn. of org. compd. to suspn. of Pd-complex (CH2Cl2) using n-Bu4NI as phase transfer catalyst and stirring. The yellow suspn. is dissolved within 5 min.; | 85% |
In dichloromethane Addn. of org. compd. to suspn. of Pd-complex (CH2Cl2). After stirring of mixt. (10 min), the yellow suspn. comes into soln. and some white solid is pptd. Further stirring for 1 h.; Washing 3 times with H2O, removal of solvent, recrystn. of residue from n-hexane/CH2Cl2, elem. anal.; | 63% |
ammonium O,O-diethyldithiophosphate
dichlorodiethylstannane
(C2H5)2SnCl(SSP(OC2H5)2)
Conditions | Yield |
---|---|
In hexane byproducts: NH4Cl; to a susp. of NH4SSP(OEt)2 in hexane a soln. of Et2SnCl2 was added in 1:1 stoich. and the reaction mixt. was allowed to stir for 2-3 h at roomtemp; NH4Cl formed during the reaction was filtered off, filtrate was concd. under vac., elem. anal.; | 85% |
ammonium O,O-diethyldithiophosphate
chlorotriphenylgermane
triphenyl(O,O'-diethyldithiophosphato)germanium
Conditions | Yield |
---|---|
In benzene byproducts: NH4Cl; soln. of 1.0 mmol of Ph3GeCl and C6H6 added to 1.2 mmol of dry (EtO)2PS(S)NH4 under dry N2, warmed up to 20°C, stirred for 4 h; NH4Cl filtered off, filtrate slowly evapd. in vac.; elem. anal.; | 85% |
ammonium O,O-diethyldithiophosphate
dibutyltin chloride
dibutyltin(IV) diethyldithiophosphate
Conditions | Yield |
---|---|
In benzene byproducts: NH4Cl; to suspn. of ammonium diethyldithiophosphate is added dialkyltindichloride in benzene, exothermic reaction, white ppt. separates at room temp.,refluxing for 0.5 h; ppt. is filtered off, benzene is removed under reduced pressure, distn.(100-102°C/0.01 mm), elem. anal.; | 85% |
In benzene byproducts: NH4Cl; to suspn. of ammonium diethyldithiophosphate is added dialkyltindichloride in benzene, exothermic reaction, white ppt. separates at room temp.,refluxing for 0.5 h; ppt. is filtered off, benzene is removed under reduced pressure, distn., elem. anal.; | 80% |
ammonium O,O-diethyldithiophosphate
[Mo(η(5)-cyclopentadienyl)Cl2(O,O'-diethyldithiophosphate)]
Conditions | Yield |
---|---|
In dichloromethane under N2 atm. using Schlenk techniques; to suspn. of Mo complex in CH2Cl2 added org. salt at room temp.; stirred for 10 h; mixt. filtered; filtrate concd. to dryness; residue washed (Et2O); elem.anal.; | 85% |
ammonium O,O-diethyldithiophosphate
trichloro(2,2'-bipyridine)ruthenium
Ru((C5H4N)2)(SP(S)(OC2H5)2)2
Conditions | Yield |
---|---|
In methanol elem. anal.; | 85% |
ammonium O,O-diethyldithiophosphate
Conditions | Yield |
---|---|
In dichloromethane suspn. of Pd complex and protic ligand (1:2) in CH2Cl2 stirred at room temp. for 30 min; concd.(vac.), pptd.(Et2O), filtered, washed (H2O, Et2O), dried (air), recrystd.(CH2Cl2/Et2O), elem. anal.; | 84% |
ammonium O,O-diethyldithiophosphate
MoI2(CO)3(MeCN)2
triphenylphosphine
Mo(CO)2(S2P(OC2H5)2)2(P(C6H5)3)
Conditions | Yield |
---|---|
In dichloromethane byproducts: CO; MoI2(CO)3(NCMe)2 dissolved in CH2Cl2; solid NH4(S2P(OEt)2) added with stirring; after 30 min ppt. filtered off; to filtrate PPh3 added; soln. stirred for 30 min; concd.; hexane added; cooled down (-20°C) overnight; elem. anal.; | 83% |
ammonium O,O-diethyldithiophosphate
tetrakis(actonitrile)copper(I) hexafluorophosphate
Conditions | Yield |
---|---|
In tetrahydrofuran under inert atm. soln. Cu(MeCN)4PF6, NH4(S2P(O-i-Pr)2), and NaBD4 in THFwere stirred at room temp. for 30 min; soln. was filtered and evapd. to dryness in vacuo, residue was washed with water and dried in vacuo; elem. anal.; | 83% |
ammonium O,O-diethyldithiophosphate
tetrakis(actonitrile)copper(I) hexafluorophosphate
Conditions | Yield |
---|---|
In acetone byproducts: NH4PF6; under inert atm. soln. Cu(MeCN)4PF6 and NH4(S2P(OEt)2) in acetone was stirred at room temp. for 1 h; soln. was filtered and evapd. to dryness in vacuo, residue was washed with water; elem. anal.; | 83% |
ammonium O,O-diethyldithiophosphate
diphenyltin(IV) dichloride
(C6H5)2SnCl(SSP(OC2H5)2)
Conditions | Yield |
---|---|
In hexane byproducts: NH4Cl; to a susp. of NH4SSP(OEt)2 in hexane a soln. of Ph2SnCl2 was added in 1:1 stoich. and the reaction mixt. was allowed to stir for 2-3 h at roomtemp; NH4Cl formed during the reaction was filtered off, filtrate was concd. under vac., elem. anal.; | 82% |
ammonium O,O-diethyldithiophosphate
Conditions | Yield |
---|---|
In water A soln. of CuSO4 in H2O was added NH4S2P(OR)2 in H2O; brown ppt. was extd. with CH2Cl2, evapd., MeOH was added;; ppt. was recrystd. from CH2Cl2-C6H5CH3; elem. anal.;; | 82% |
ammonium O,O-diethyldithiophosphate
dichlorodimethylgermanium
dimethylbis(O,O'-diethyldithiophosphato)germanium
Conditions | Yield |
---|---|
In benzene byproducts: NH4Cl; soln. of 1.3 mmol of Me2GeCl2 and C6H6 added to 2.8 mmol of dry (EtO)2PS(S)NH4 occasionally cooled to -10°C under dry N2, warmed up to 10°C, stirred for 4 h; NH4Cl filtered off, filtrate slowly evapd. in vac.; elem. anal.; | 82% |
ammonium O,O-diethyldithiophosphate
[W(acetonitrile)2(η3-allyl)(CO)2Br]
[W(acetonitrile)(η3-allyl)(CO)2(η2-diethyldithiophosphato)]
Conditions | Yield |
---|---|
In dichloromethane under N2; CH2Cl2 added to equimolar mixt. of W complex and ligand at ambient temp.; stirred for 10 min; solvent removed in vac.; abstracted with Et2O; n-hexane added; filtered;ppt. washed with cold n-hexane; dried in vac.; recrystd. from cold n-he xane-Et2O; elem. anal.; | 82% |
tetrahydrofuran
sodium tetrahydroborate
ammonium O,O-diethyldithiophosphate
tetrakis(actonitrile)copper(I) hexafluorophosphate
Conditions | Yield |
---|---|
In tetrahydrofuran under inert atm. soln. Cu(MeCN)4PF6, NH4(S2P(OEt)2), and NaBH4 in THF were stirred at room temp. for 30 min; soln. was filtered and evapd. to dryness in vacuo, residue was washed with water and dried in vacuo; elem. anal.; | 82% |
ammonium O,O-diethyldithiophosphate
(C5(CH3)5)RhCl(S2P(OC2H5)2)
Conditions | Yield |
---|---|
In dichloromethane byproducts: NH4Cl; N2-atmosphere; stoich. amts., stirring (room temp., 3 h); filtration off of NH4Cl, concn. (vac.), recrystn. (CH2Cl2/hexane); elem. anal.; | 81% |
ammonium O,O-diethyldithiophosphate
MoI2(CO)3(MeCN)2
1,2-bis-(diphenylphosphino)ethane
MoI(CO)2((C6H5)2PCH2)2(S2P(OC2H5)2)
Conditions | Yield |
---|---|
In dichloromethane MoI2(CO)3(NCMe)2 dissolved in CH2Cl2; NH4(S2P(OEt)2) added with stirring; after 30 min mixt. filtered; Ph2PCH2CH2PPh2 added to filtrate; soln. stirred for 30 min; hexane added; mixt. kept at 0.°C for 3 ds; elem. anal.; | 81% |
sodium tetrahydroborate
ammonium O,O-diethyldithiophosphate
Conditions | Yield |
---|---|
In chloroform at 20℃; for 1h; Inert atmosphere; Schlenk technique; | 81% |
Empirical Formula: C4H14NO2PS2
Molecular Weight: 203.2632
Flash Point: 94.5 °C
Enthalpy of Vaporization: 45.03 kJ/mol
Boiling Point: 232.7 °C at 760 mmHg
Vapour Pressure: 0.0887 mmHg at 25 °C
Melting point: 164-166 °C(lit.)
Appearance: White powder
Structure of Ammonium O,O-diethyl dithiophosphate (CAS NO.1068-22-0):
IUPAC Name: Azanium diethoxy-sulfanylidene-sulfido-λ5-phosphane
Canonical SMILES: CCOP(=S)(OCC)[S-].[NH4+]
InChI: InChI=1S/C4H11O2PS2.H3N/c1-3-5-7(8,9)6-4-2;/h3-4H2,1-2H3,(H,8,9);1H3
InChIKey: HFRHTRKMBOQLLL-UHFFFAOYSA-N
Product Category of Ammonium O,O-diethyl dithiophosphate (CAS NO.1068-22-0): Pharmaceutical Intermediates;Organic Building Blocks;Organic Phosphates/Phosphites;Phosphorus Compounds
1. | skn-rbt 500 mg MLD | 34ZIAG Toxicology of Drugs and Chemicals ,Deichmann, W.B.,New York, NY.: Academic Press, Inc.,1969,97. | ||
2. | eye-rbt 100 mg MLD | 34ZIAG Toxicology of Drugs and Chemicals ,Deichmann, W.B.,New York, NY.: Academic Press, Inc.,1969,97. | ||
3. | orl-rat LD50:7900 mg/kg | 34ZIAG Toxicology of Drugs and Chemicals ,Deichmann, W.B.,New York, NY.: Academic Press, Inc.,1969,97. |
Mildly toxic by ingestion. An eye and skin irritant. When heated to decomposition it emits toxic fumes of POx, SOx, NH3, and NOx.
Hazard Codes: Xn
Risk Statements: 20/21/22
R20/21/22:Harmful by inhalation, in contact with skin and if swallowed.
Safety Statements: 36
S36:Wear suitable protective clothing.
Ammonium O,O-diethyl dithiophosphate , its cas register number is 1068-22-0. It also can be called Phosphorodithioic acid, O,O-diethyl ester, ammonium salt ; S-Ammonium O,O'-diethyl phosphorodithioate ; and Ammonium ethyl phosphorodithioate (6CI,7CI) . It is hazardous, so the first aid measures and others should be known. Such as: When on the skin: first, should flush skin with plenty of water immediately for at least 15 minutes while removing contaminated clothing. Secondly, get medical aid. Or in the eyes: Flush eyes with plenty of water for at least 15 minutes, occasionally lifting the upper and lower eyelids. Then get medical aid soon. While, it's inhaled: Remove from exposure and move to fresh air immediately. Then you have the ingesting of the product: Wash mouth out with water, and get medical aid immediately.
In addition, Ammonium O,O-diethyl dithiophosphate (CAS NO.1068-22-0) could be stable under normal temperatures and pressures. It is not compatible with strong oxidants. And also prevent it to broken down into hazardous decomposition products: irritating and toxic fumes and gases.
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