Dichloromethane → 2-Pyrrolidinone, 3-chloro-4-(chloromethyl)-1-(phenylmethyl)-

HRID 1111861ノート

反応式

HRID 1111861 の反応式
[CH2:1]([N:4]([CH2:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1)[C:5](=[O:9])[CH:6](Cl)[Cl:7])[CH:2]=[CH2:3].COCCOCCOC.N1CCCC1=O.C(Cl)[Cl:33]>>[CH2:10]([N:4]1[CH2:1][CH:2]([CH2:3][Cl:33])[CH:6]([Cl:7])[C:5]1=[O:9])[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1

参加物

5

実験手順

Eleven and one-tenth grams of N-allyl-N-benzyl dichloroacetamide was dissolved in 12 ml. of diglyme and 1 g. of anhydrous ferrous chloride added. The mixture was heated at reflux under nitrogen until conversion to the pyrrolidinone was complete as indicated by GLPC. The mixture was diluted with methylene chloride, washed with 5 percent hydrochloric acid, separated, dried over anhydrous magnesium sulfate, treated with activated carbon and Florisil and stripped under vacuum. Yield was 6 g. of the title compound, nD30 1.5387.

後処理

  1. temperatureThe mixture was heated
  2. washwashed with 5 percent hydrochloric acid
  3. customseparated
  4. dry with materialdried over anhydrous magnesium sulfate
  5. additiontreated with activated carbon and Florisil

出典と根拠

ORDレコード
ord-5f883e302c4a4256a63feae086771481
出典データセット
uspto-grants-1978_10
特許番号
US04119636

反応ノート

読み込み中…