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perchloric acid
water
sodium hydrogencarbonate
sodium perchlorate monohydrate
Conditions | Yield |
---|---|
In perchloric acid by a react. of HClO4 with NaHCO3; evapn. to incipient crystn.; |
sodium perchlorate monohydrate
Conditions | Yield |
---|---|
In water crystn. below 52.75°C; | |
In water crystn. below 52.75°C; |
Conditions | Yield |
---|---|
In not given neutralization, concg. to satn. concn., hot filtration, cooling the filtrate at stirring; recrystn. from water twice; | |
In perchloric acid dissoln. of carbonate in HClO4 (72 %), repeated recrystn. (H2O); | |
In not given neutralization, concg. to satn. concn., hot filtration, cooling the filtrate at stirring; recrystn. from water twice, washing by dry ether, drying in vac. for 10 h at ambient temp.; | |
In not given neutralization, concg. to satn. concn., hot filtration, cooling the filtrate at stirring; recrystn. from water twice; | |
In not given neutralization, concg. to satn. concn., hot filtration, cooling the filtrate at stirring; recrystn. from water twice, washing by dry ether, drying in vac. for 10 h at ambient temp.; |
Conditions | Yield |
---|---|
With aq. HClO4 dry box.; |
sodium perchlorate monohydrate
{(NH3)5IrOCHN(CH3)2}(3+)*3ClO4(1-)={(NH3)5IrOCHN(CH3)2}(ClO4)3
{(NH3)5IrOOCH}(2+)*2ClO4(1-)={(NH3)5IrOOCH}(ClO4)2
Conditions | Yield |
---|---|
With sodium hydroxide In water Kinetics; stirred for 10 min at ambient temp., NaClO4*H2O was added in H2O; cooled, filtered, elem. anal.; | 100% |
sodium perchlorate monohydrate
[Pd(η3-1,1,2-Me3C3H2)(2-isopropylthiomethylpyridine)](ClO4)
Conditions | Yield |
---|---|
In methanol; dichloromethane stirred at room temp. under N2 for 1 h; evapd. in vacuo, residue dissolved in CH2Cl2, treated with activated charcoal, filtered through celite, filtrate was concd., treated with Et2O, ppt. was collected; elem. anal.; | 99% |
Conditions | Yield |
---|---|
In water at 20℃; for 2h; Sealed tube; | 99% |
sodium perchlorate monohydrate
Conditions | Yield |
---|---|
In not given to Pt-salt NaClO4*H2O added; filtered, washed (H2O), dried in vac., elem. anal.; | 98% |
Conditions | Yield |
---|---|
In acetonitrile equimol., a soln. of salt added to a soln. of S compd., stirred overnight at room temp.; solvent evapd., residue washed (cold diethyl ether), dried (vac.); elem.anal.; | 98% |
Conditions | Yield |
---|---|
Stage #1: C21H24N3Pd(1+)*ClO4(1-); triphenylphosphine In dichloromethane for 0.166667h; Inert atmosphere; Schlenk technique; Stage #2: sodium perchlorate monohydrate In dichloromethane at 20℃; for 1h; Inert atmosphere; Schlenk technique; | 98% |
Conditions | Yield |
---|---|
In methanol; dichloromethane at 20℃; for 0.5h; Inert atmosphere; Schlenk technique; | 98% |
sodium perchlorate monohydrate
2-<(phenylseleno)methyl>pyridine
Conditions | Yield |
---|---|
In dichloromethane mixed, stirred for 30 min; concd.(vac.), treated with activated charcoal in CH2Cl2, filtered, conctd., pptd.(diethyl ether), elem. anal., IR, NMR; | 97.6% |
sodium perchlorate monohydrate
bis(μ-chloro)bis{(1,2,3-η)-3-methyl-2-butenyl}palladium
Pd(II)(η1,1-dimethyl-C3H3)(C5H3CH3NCH2SC6H5) perchlorate
Conditions | Yield |
---|---|
In dichloromethane mixed, stirred for 30 min; concd.(vac.), treated with activated charcoal in CH2Cl2, filtered, conctd., pptd.(diethyl ether), elem. anal., IR, NMR; | 97.3% |
sodium perchlorate monohydrate
[Au(C6H4N2C6H5)Cl2]
Conditions | Yield |
---|---|
With pyridine In acetone byproducts: NaCl; stirring (1 h, room temp.); evapn., extn. (CH2Cl2), filtration, concn., pptn. on Et2O addn., recrystn. (CH2Cl2/Et2O); elem. anal.; | 97% |
Conditions | Yield |
---|---|
In methanol; dichloromethane byproducts: NaCl; addn. of soln. of P compd. in CH2Cl2 to soln. of Pd complex in CH2Cl2, addn. of soln. of Na compd. in MeOH; filtration, stirring (30 min), evapn., dissolving in CH2Cl2, treatment with activated charcoal, filtration (Celite), concn. under reduced pressure, addn. of Et2O, filtration, washing with Et2O and n-pentane, drying under vacuum, elem. anal.; | 97% |
sodium perchlorate monohydrate
2,6-dimethylphenyl isonitrile
triphenylphosphine
[Pd(2,6-dimethylphenylisocyanide)(triphenylphosphine)(allyl)]ClO4
Conditions | Yield |
---|---|
In methanol; dichloromethane byproducts: NaCl; addn. of soln. of N compd. in CH2Cl2 to soln. of Pd complex in CH2Cl2, addn. of soln. of PPh3 in CH2Cl2, addn. of Na compd. in MeOH; filtration, stirring (30 min), evapn. under reduced pressure, dissolvingin CH2Cl2, treatment with charcoal, filtration (Celite), concn. under r educed pressure, addn. of Et2O, filtration, washing (Et2O, pentane), drying under vacuum, elem. anal.; | 97% |
N,N-bis(-pyridin-2ylmethyl)benzenamine
dichloro bis(acetonitrile) palladium(II)
sodium perchlorate monohydrate
N,N-di(2-picolyl)aniline(chloro)PdII perchlorate
Conditions | Yield |
---|---|
In ethanol at 20℃; for 12h; | 96.8% |
sodium perchlorate monohydrate
Conditions | Yield |
---|---|
With P(C6H5)3 In methanol; dichloromethane Pd complex treated with PPh3; NaClO4*H2O added to the soln.; stirring for 10 min; evapn.; extn. with CH2Cl2 and charcoal; filtration; concn.; addn. of Et2O; elem. anal.; | 96.3% |
sodium perchlorate monohydrate
2-(phenyl-selenomethyl)-6-methyl-pyridine
Conditions | Yield |
---|---|
In dichloromethane mixed, stirred for 30 min; concd.(vac.), treated with activated charcoal in CH2Cl2, filtered, conctd., pptd.(diethyl ether), elem. anal., IR, NMR; | 96.2% |
perchloric acid
water
sodium hydrogencarbonate
sodium perchlorate monohydrate
Conditions | Yield |
---|---|
In perchloric acid by a react. of HClO4 with NaHCO3; evapn. to incipient crystn.; |
sodium perchlorate monohydrate
Conditions | Yield |
---|---|
In water crystn. below 52.75°C; | |
In water crystn. below 52.75°C; |
Conditions | Yield |
---|---|
In not given neutralization, concg. to satn. concn., hot filtration, cooling the filtrate at stirring; recrystn. from water twice; | |
In perchloric acid dissoln. of carbonate in HClO4 (72 %), repeated recrystn. (H2O); | |
In not given neutralization, concg. to satn. concn., hot filtration, cooling the filtrate at stirring; recrystn. from water twice, washing by dry ether, drying in vac. for 10 h at ambient temp.; | |
In not given neutralization, concg. to satn. concn., hot filtration, cooling the filtrate at stirring; recrystn. from water twice; | |
In not given neutralization, concg. to satn. concn., hot filtration, cooling the filtrate at stirring; recrystn. from water twice, washing by dry ether, drying in vac. for 10 h at ambient temp.; |
Conditions | Yield |
---|---|
With aq. HClO4 dry box.; |
sodium perchlorate monohydrate
{(NH3)5IrOCHN(CH3)2}(3+)*3ClO4(1-)={(NH3)5IrOCHN(CH3)2}(ClO4)3
{(NH3)5IrOOCH}(2+)*2ClO4(1-)={(NH3)5IrOOCH}(ClO4)2
Conditions | Yield |
---|---|
With sodium hydroxide In water Kinetics; stirred for 10 min at ambient temp., NaClO4*H2O was added in H2O; cooled, filtered, elem. anal.; | 100% |
sodium perchlorate monohydrate
[Pd(η3-1,1,2-Me3C3H2)(2-isopropylthiomethylpyridine)](ClO4)
Conditions | Yield |
---|---|
In methanol; dichloromethane stirred at room temp. under N2 for 1 h; evapd. in vacuo, residue dissolved in CH2Cl2, treated with activated charcoal, filtered through celite, filtrate was concd., treated with Et2O, ppt. was collected; elem. anal.; | 99% |
Conditions | Yield |
---|---|
In water at 20℃; for 2h; Sealed tube; | 99% |
sodium perchlorate monohydrate
Conditions | Yield |
---|---|
In not given to Pt-salt NaClO4*H2O added; filtered, washed (H2O), dried in vac., elem. anal.; | 98% |
Conditions | Yield |
---|---|
In acetonitrile equimol., a soln. of salt added to a soln. of S compd., stirred overnight at room temp.; solvent evapd., residue washed (cold diethyl ether), dried (vac.); elem.anal.; | 98% |
Conditions | Yield |
---|---|
Stage #1: C21H24N3Pd(1+)*ClO4(1-); triphenylphosphine In dichloromethane for 0.166667h; Inert atmosphere; Schlenk technique; Stage #2: sodium perchlorate monohydrate In dichloromethane at 20℃; for 1h; Inert atmosphere; Schlenk technique; | 98% |
Conditions | Yield |
---|---|
In methanol; dichloromethane at 20℃; for 0.5h; Inert atmosphere; Schlenk technique; | 98% |
sodium perchlorate monohydrate
2-<(phenylseleno)methyl>pyridine
Conditions | Yield |
---|---|
In dichloromethane mixed, stirred for 30 min; concd.(vac.), treated with activated charcoal in CH2Cl2, filtered, conctd., pptd.(diethyl ether), elem. anal., IR, NMR; | 97.6% |
sodium perchlorate monohydrate
bis(μ-chloro)bis{(1,2,3-η)-3-methyl-2-butenyl}palladium
Pd(II)(η1,1-dimethyl-C3H3)(C5H3CH3NCH2SC6H5) perchlorate
Conditions | Yield |
---|---|
In dichloromethane mixed, stirred for 30 min; concd.(vac.), treated with activated charcoal in CH2Cl2, filtered, conctd., pptd.(diethyl ether), elem. anal., IR, NMR; | 97.3% |
sodium perchlorate monohydrate
[Au(C6H4N2C6H5)Cl2]
Conditions | Yield |
---|---|
With pyridine In acetone byproducts: NaCl; stirring (1 h, room temp.); evapn., extn. (CH2Cl2), filtration, concn., pptn. on Et2O addn., recrystn. (CH2Cl2/Et2O); elem. anal.; | 97% |
Conditions | Yield |
---|---|
In methanol; dichloromethane byproducts: NaCl; addn. of soln. of P compd. in CH2Cl2 to soln. of Pd complex in CH2Cl2, addn. of soln. of Na compd. in MeOH; filtration, stirring (30 min), evapn., dissolving in CH2Cl2, treatment with activated charcoal, filtration (Celite), concn. under reduced pressure, addn. of Et2O, filtration, washing with Et2O and n-pentane, drying under vacuum, elem. anal.; | 97% |
sodium perchlorate monohydrate
2,6-dimethylphenyl isonitrile
triphenylphosphine
[Pd(2,6-dimethylphenylisocyanide)(triphenylphosphine)(allyl)]ClO4
Conditions | Yield |
---|---|
In methanol; dichloromethane byproducts: NaCl; addn. of soln. of N compd. in CH2Cl2 to soln. of Pd complex in CH2Cl2, addn. of soln. of PPh3 in CH2Cl2, addn. of Na compd. in MeOH; filtration, stirring (30 min), evapn. under reduced pressure, dissolvingin CH2Cl2, treatment with charcoal, filtration (Celite), concn. under r educed pressure, addn. of Et2O, filtration, washing (Et2O, pentane), drying under vacuum, elem. anal.; | 97% |
N,N-bis(-pyridin-2ylmethyl)benzenamine
dichloro bis(acetonitrile) palladium(II)
sodium perchlorate monohydrate
N,N-di(2-picolyl)aniline(chloro)PdII perchlorate
Conditions | Yield |
---|---|
In ethanol at 20℃; for 12h; | 96.8% |
sodium perchlorate monohydrate
Conditions | Yield |
---|---|
With P(C6H5)3 In methanol; dichloromethane Pd complex treated with PPh3; NaClO4*H2O added to the soln.; stirring for 10 min; evapn.; extn. with CH2Cl2 and charcoal; filtration; concn.; addn. of Et2O; elem. anal.; | 96.3% |
sodium perchlorate monohydrate
2-(phenyl-selenomethyl)-6-methyl-pyridine
Conditions | Yield |
---|---|
In dichloromethane mixed, stirred for 30 min; concd.(vac.), treated with activated charcoal in CH2Cl2, filtered, conctd., pptd.(diethyl ether), elem. anal., IR, NMR; | 96.2% |
sodium perchlorate monohydrate
2-(phenyl-selenomethyl)-6-methyl-pyridine
Conditions | Yield |
---|---|
In dichloromethane mixed, stirred for 30 min; concd.(vac.), treated with activated charcoal in CH2Cl2, filtered, conctd., pptd.(diethyl ether), elem. anal., IR, NMR; | 96% |
sodium perchlorate monohydrate
2,2',2''-triaminotriethylamine
1,4-dimethoxybenzene-2,6-dicarboxaldehyde
Conditions | Yield |
---|---|
In ethanol addn. of the amine in EtOH to the dialdehyde and AgNO3 in EtOH, stirring, filtration, addn. of excess NaClO4*H2O in EtOH; elem. anal.; | 96% |
Conditions | Yield |
---|---|
Stage #1: pyridine; [Pt(phpytabn)Cl] In methanol; acetonitrile at 60℃; for 0.75h; Stage #2: sodium perchlorate monohydrate at 20℃; for 0.5h; | 96% |
sodium perchlorate monohydrate
Conditions | Yield |
---|---|
With P(C6H5)3 In methanol; dichloromethane Pd complex treated with PPh3; NaClO4*H2O added to the soln.; stirring for 10 min; evapn.; extn. with CH2Cl2 and charcoal; filtration; concn.; addn. of Et2O; elem. anal.; | 95.7% |
sodium perchlorate monohydrate
2-[(phenylsulfanyl)methyl]pyridine
Pd(II)(η3-1-phenyl-C3H4)(C5H3CH3NCH2SC6H5) perchlorate
Conditions | Yield |
---|---|
In dichloromethane mixed, stirred for 30 min; concd.(vac.), treated with activated charcoal in CH2Cl2, filtered, conctd., pptd.(diethyl ether), elem. anal., IR, NMR; | 95.3% |
sodium perchlorate monohydrate
dimethyl sulfate
PdCl(P(C6H5)3)2C5H3NCH3Cl(1+)*ClO4(1-)=(PdCl(P(C6H5)3)2C5H3NCH3Cl)ClO4
Conditions | Yield |
---|---|
In dichloromethane reflux for 4 h, standing overnight at room temp., concn., pptn. with Et2O, dissoln. in CH2Cl2, addn. of NaClO4*H2O in MeOH; stirring for 10 min;; evapn., extn. with CH2Cl2 and charcoal, filtn., concn. and pptn. with Et2O, elem. anal.;; | 95% |
sodium perchlorate monohydrate
bis(1,4,7-trithiacyclononane)cobalt(II) bisperchlorate
[Co(1,4,7-trithiacyclononane)2](ClO4)3
Conditions | Yield |
---|---|
With Na2S2O8 In water a soln. of Na2S2O8 added to a soln. of Co-complex; NaClO4*H2O added; pptd.; filtered; washed with ethanol and water; air-dried; elem. anal.; | 95% |
sodium perchlorate monohydrate
Conditions | Yield |
---|---|
In methanol addn. of methanolic soln. of NaClO4 to methanolic soln. of Pd compd., stirred for 12 h at ambient temp.; evapn., extn. (CH2Cl2), concn., diln. (hexane); elem. anal.; | 95% |
sodium perchlorate monohydrate
Pd(II)(η1-phenyl-C3H4)(C5H4NCH2SC6H5) perchlorate
Conditions | Yield |
---|---|
In dichloromethane mixed, stirred for 30 min; concd.(vac.), treated with activated charcoal in CH2Cl2, filtered, conctd., pptd.(diethyl ether), elem. anal., IR, NMR; | 95% |
sodium perchlorate monohydrate
2,6-dimethylphenyl isonitrile
Conditions | Yield |
---|---|
In methanol; dichloromethane byproducts: NaCl; addn. of soln. of CNC6H3Me2 in CH2Cl2 to Pd complex in CH2Cl2, addn. of soln. of Na compd. in MeOH; filtration, stirring for 30 min, evapn. under reduced pressure, dissolving in CH2Cl2, treatment with activated charcoal, filtration (Celite), concn., pptn. by addn. of Et2O, filtration, washing (Et2O, pentane), drying under vacuum, elem. anal.; | 95% |
sodium perchlorate monohydrate
2,6-dimethylphenyl isonitrile
Conditions | Yield |
---|---|
In methanol; dichloromethane byproducts: NaCl; addn. of soln. of CNC6H3Me2 in CH2Cl2 to Pd complex in CH2Cl2, addn. of soln. of Na compd. in MeOH; filtration, stirring for 30 min, evapn. under reduced pressure, dissolving in CH2Cl2, treatment with activated charcoal, filtration (Celite), concn., pptn. by addn. of Et2O, filtration, washing (Et2O, pentane), drying under vacuum, elem. anal.; | 95% |
sodium perchlorate monohydrate
Conditions | Yield |
---|---|
Stage #1: (2-methylallyl)palladium-chloride dimer; ([1-(phenylthio)methylene-3-mesityl]imidazolyl-2-ene)silverbromide In dichloromethane at 20℃; Inert atmosphere; Stage #2: sodium perchlorate monohydrate In methanol; dichloromethane Inert atmosphere; | 95% |
sodium perchlorate monohydrate
bis(μ-chloro)bis{(1,2,3-η)-3-methyl-2-butenyl}palladium
2-<(phenylseleno)methyl>pyridine
Conditions | Yield |
---|---|
In dichloromethane mixed, stirred for 30 min; concd.(vac.), treated with activated charcoal in CH2Cl2, filtered, conctd., pptd.(diethyl ether), elem. anal., IR, NMR; | 94.7% |
sodium perchlorate monohydrate
chloroacetone
cis-{PdCl((1-CH2COMe)C5H4N-C2)(dppe)}ClO4
Conditions | Yield |
---|---|
In acetone Kinetics; reaction with excess chloride; stirred for 24 h at ambient temp.; addn. of perchlorate;; evapn.; extn. (CH2Cl2, charcoal); filtration; concn.; pptn. by addn. of Et2O; repptn. from CH2Cl2/Et2O; elem. anal.; | 94.4% |
dichloro bis(acetonitrile) palladium(II)
sodium perchlorate monohydrate
N,N-di(2-picolyl)benzylamine
N,N-di(2-picolyl)benzylamine(chloro)PdII perchlorate
Conditions | Yield |
---|---|
In ethanol at 20℃; for 12h; | 94.2% |
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