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Diethylamine → HCID 13504017, 화합물

HRID 1165878
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HRID 1165878 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

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

생성물 1

HCID 13504017HCID 13504017, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-6a29b0c3761a4f4b8f81c0085cff61bc
출처 데이터셋
uspto-grants-1990_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04912129

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