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

HRID 1834108

Reaktionsgleichung

Reaktionsgleichung von HRID 1834108
[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]

Komponenten

4

Edukt 3

HCID 6344DichloromethaneHCID 8150DiglymeHCID 37829Dichlormid

Produkt 1

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

Versuchsvorschrift

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.

Aufarbeitung

  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

Quellen und Nachweise

ORD-Eintrag
ord-af3b3c93f60243b5abe0e4a934306a62
Quelldatensatz
uspto-grants-1978_01
Patentnummer
US04069038

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