Butyl Chloride → 1-Diazopentan-2-one

HRID 648227

反応式

HRID 648227 の反応式
[CH3:1][N:2]([N:6]=O)[C:3](N)=[O:4].[N+:8](=[CH2:10])=[N-:9].[CH3:11][CH2:12][O:13][CH2:14][CH3:15].[CH2:16](Cl)[CH2:17][CH2:18]C>>[N+:2](=[CH2:1])=[N-:6].[CH3:11][CH2:12][O:13][CH2:14][CH3:15].[N+:8](=[CH:10][C:3](=[O:4])[CH2:16][CH2:17][CH3:18])=[N-:9]

参加物

5

反応物 3

HCID 8005Butyl ChlorideHCID 12699N-Methyl-N-nitrosoureaHCID 21186548Diazomethane diethylether

生成物 2

HCID 21186548Diazomethane diethyletherHCID 537665711-Diazopentan-2-one収率 97.8%

実験手順

A 100 ml quantity of diazomethane ether solution (containing 2.8 g of diazomethane) is prepared from 10 g of N-methyl-N-nitrosourea. To the diazomethane ether solution is added dropwise 1.7 g of n-butyl chloride with ice-cooling, and the mixture is thereafter stirred for 30 minutes. Nitrogen gas is passed through the reaction mixture at room temperature to remove the excess of diazomethane therefrom. The ethereal solution is distilled in a vacuum, and the residue is purified by column chromatography (silica gel, developed with chloroform) to give 1.75 g of light yellow oily 1-diazo-2-pentanone (yield 97.8%).

後処理

  1. temperaturecooling
  2. customis passed through the reaction mixture at room temperature
  3. customto remove the excess of diazomethane
  4. distillationThe ethereal solution is distilled in a vacuum
  5. customthe residue is purified by column chromatography (silica gel, developed with chloroform)

出典と根拠

ORDレコード
ord-ca904204424848a9bda228488484210c
出典データセット
uspto-grants-1983_10
特許番号
US04411911

関連ノート

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