Dichloromethane → HCID 13295673、化合物

HRID 1111860

反応式

HRID 1111860 の反応式
[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]

参加物

4

反応物 3

HCID 6344DichloromethaneHCID 8150DiglymeHCID 37829Dichlormid

生成物 1

HCID 13295673HCID 13295673、化合物

実験手順

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 (FeCl2.4H2O) 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 (FeCl2.4H2O) 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.

後処理

  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

出典と根拠

ORDレコード
ord-9fedb49c30f64293990994ae3ba5cc19
出典データセット
uspto-grants-1978_10
特許番号
US04119636

関連ノート

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