Butyl Chloride → 1-Diazopentan-2-one

HRID 648227

반응식

HRID 648227 반응식
[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]

참가 물질

5

반응물 3

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

생성물 2

HCID 21186548Diazomethane diethyletherHCID 537665711-Diazopentan-2-one수율 97.8%

실험 절차

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%).

후처리

  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)

출처 및 근거

ORD 기록
ord-ca904204424848a9bda228488484210c
출처 데이터셋
uspto-grants-1983_10
특허 번호
US04411911

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