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

HRID 1395394
ノート
印刷プレビュー

反応式

HRID 1395394 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 66133Benzyl triethylammonium chloride
触媒
HCID 6344Dichloromethane溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-a6ef4567212946678b0b7496963aeee6
出典データセット
uspto-grants-1980_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04203932

反応ノート

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