Dichloromethane → 3-Chloro-4-(chloromethyl)-1-prop-2-enylpyrrolidin-2-one

HRID 1834108

반응식

HRID 1834108 반응식
[CH2:1]([N:4]([CH2:10][CH:11]=[CH2:12])[C:5](=[O:9])[CH:6](Cl)[Cl:7])[CH:2]=[CH2:3].COCCOCCOC.C(Cl)[Cl:23]>>[CH2:1]([N:4]1[CH2:10][CH:11]([CH2:12][Cl:23])[CH:6]([Cl:7])[C:5]1=[O:9])[CH:2]=[CH2:3]

참가 물질

4

반응물 3

HCID 6344DichloromethaneHCID 8150DiglymeHCID 37829Dichlormid

생성물 1

HCID 132956733-Chloro-4-(chloromethyl)-1-prop-2-enylpyrrolidin-2-one

실험 절차

Twenty and eight-tenths grams of N,N-diallyl dichloroacetamide was mixed with 25 g. of diethylene glycol dimethyl ether (diglyme), 1 g. of ferrous chloride (FeC12 ·4H2 0) added and the mixture was heated at reflux for 30 minutes. The conversion was monitored by the appearance of a new carbonyl peak at ~ 5.8 microns in the infrared. An additional gram of ferrous chloride (FeC12 ·4H2 0) was added and heating was continued for an additional 30 minutes. The reaction mixture was diluted with methylene chloride, washed with water and dried and stripped. The dark liquid product was distilled under vacuum to give 8.4 g. of light yellow oil, b.p. 124°-127° C. at 0.25 mm. nD30 1.4850.

후처리

  1. temperaturethe mixture was heated
  2. temperatureat reflux for 30 minutes
  3. temperatureheating
  4. washwashed with water
  5. customdried
  6. distillationThe dark liquid product was distilled under vacuum
  7. customto give 8.4 g

출처 및 근거

ORD 기록
ord-af3b3c93f60243b5abe0e4a934306a62
출처 데이터셋
uspto-grants-1978_01
특허 번호
US04069038

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