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Carbon Tetrachloride → 1-Acetyl-1-Methyl-2-Diethoxyphosphoryl Hydrazine

HRID 1395394
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HRID 1395394 반응식
[C:1]([N:4]([CH3:6])[NH2:5])(=[O:3])[CH3:2].C(=O)([O-])[O-].[K+].[K+].C(Cl)(Cl)(Cl)Cl.[CH2:18]([O:20][P:21]([O-:25])[O:22][CH2:23][CH3:24])[CH3:19]>[Cl-].C([N+](CC)(CC)CC1C=CC=CC=1)C.ClCCl>[C:1]([N:4]([CH3:6])[NH:5][P:21]([O:22][CH2:23][CH3:24])([O:20][CH2:18][CH3:19])=[O:25])(=[O:3])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 5943Carbon TetrachlorideHCID 11430Potassium CarbonateHCID 19051Acetic acid, 1-methylhydrazideHCID 3780918Diethylphosphite

생성물 1

HCID 203392921-Acetyl-1-Methyl-2-Diethoxyphosphoryl Hydrazine

시약·촉매·용매 2

HCID 66133Benzyl triethylammonium chloride
촉매
HCID 6344Dichloromethane용매2회

실험 절차

A mixture of 1-acetyl-1-methyl hydrazine (7.84 g., 0.09 mole), potassium carbonate (18.44 g., 0.13 mole) and triethylbenzyl ammonium chloride (0.2 g,) was stirred vigorously at reflux with dichloromethane (90 ml) and carbon tetrachloride (55 ml) for 30 minutes. A solution of diethylphosphite (12.29 g, 0.09 mole) in dichloromethane (18 ml) was then added dropwise to this refluxing mixture and the mixture stirred and refluxed for an additional 20 hours. The mixture was then filtered and the filtrate dried over anhydrous magnesium sulfate. The dried filtrate, then was evaporated down to an oil which was subjected to high vacuum for 2 or 3 hours to yield a liquid product, characterized by proton NMR, infra-red and mass spectroscopy as the subject compound.

후처리

  1. stirringthe mixture stirred
  2. temperaturerefluxed for an additional 20 hours
  3. filtrationThe mixture was then filtered
  4. dry with materialthe filtrate dried over anhydrous magnesium sulfate
  5. customThe dried filtrate, then was evaporated down to an oil which
  6. customwas subjected to high vacuum for 2 or 3 hours
  7. customto yield a liquid product

출처 및 근거

ORD 기록
ord-a6ef4567212946678b0b7496963aeee6
출처 데이터셋
uspto-grants-1980_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04203932

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