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Diethylamine → HCID 13504017、化合物

HRID 1461133
ノート
印刷プレビュー

反応式

HRID 1461133 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

A mixture of 14 g (0.06 mol) of crude 1-benzyl-4-chloromethyl-pyrrolidin-2-one, prepared as in Example 1(a), 10 g of diethylamine and 50 ml of dimethylformamide was stirred or shaken for 2 hours at 150° C. in an autoclave. The reaction mixture was evaporated to dryness in vacuo, the residue was taken up in methylene chloride, and the solution was washed first with water and finally the title compound was extracted twice with 25 ml of 2 N HCl. The aqueous phase was separated, made alkaline with sodium hydroxide and the organic base was extracted with methylene chloride. The methylene chloride phase was evaporated, and the residue was distilled in vacuo. Yield: 10 g (61% of theory), bp0.05 =155°-158° C.

後処理

  1. stirringshaken for 2 hours at 150° C. in an autoclave
  2. customThe reaction mixture was evaporated to dryness in vacuo
  3. washthe solution was washed first with water
  4. extractionfinally the title compound was extracted twice with 25 ml of 2 N HCl
  5. customThe aqueous phase was separated
  6. extractionthe organic base was extracted with methylene chloride
  7. customThe methylene chloride phase was evaporated
  8. distillationthe residue was distilled in vacuo
  9. customYield: 10 g (61% of theory), bp0.05 =155°-158° C.

出典と根拠

ORDレコード
ord-8ff175480ca7447dbbd553bfde879b3e
出典データセット
uspto-grants-1991_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05073671

反応ノート

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