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Diethylamine → HCID 13504017、化合物

HRID 1165878
ノート
印刷プレビュー

反応式

HRID 1165878 の反応式
[CH2:1]([N:8]1[CH2:12][CH:11]([CH2:13]Cl)[CH2:10][C:9]1=[O:15])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH2:16]([NH:18][CH2:19][CH3:20])[CH3:17]>CN(C)C=O>[CH2:1]([N:8]1[CH2:12][CH:11]([CH2:13][N:18]([CH2:19][CH3:20])[CH2:16][CH3:17])[CH2:10][C:9]1=[O:15])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 8021DiethylamineHCID 135040151-Benzyl-4-chloromethyl-pyrrolidin-2-one

生成物 1

HCID 13504017HCID 13504017、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

14 g (0.06 mol) of crude 1-benzyl-4-chloromethyl-pyrrolidin-2-one, prepared as in Example 1a), 10 g of diethylamine and 50 ml of dimethylformamide are stirred or shaken for 2 hours at 150° C. in the autoclave. The mixture is evaporated to dryness in vacuo and the residue is taken up in methylene chloride then washed first with water and finally the title compound is extracted twice with 25 ml of 2N HCl. The aqueous phase is removed, made alkaline with sodium hydroxide solution and the organic base is extracted with methylene chloride. The methylene chloride phase is concentrated by evaporation and the residue is distilled in vacuo.

後処理

  1. stirringshaken for 2 hours at 150° C. in the autoclave
  2. customThe mixture is evaporated to dryness in vacuo
  3. washthen washed first with water
  4. extractionfinally the title compound is extracted twice with 25 ml of 2N HCl
  5. customThe aqueous phase is removed
  6. extractionthe organic base is extracted with methylene chloride
  7. concentrationThe methylene chloride phase is concentrated by evaporation
  8. distillationthe residue is distilled in vacuo

出典と根拠

ORDレコード
ord-6a29b0c3761a4f4b8f81c0085cff61bc
出典データセット
uspto-grants-1990_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04912129

反応ノート

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