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Diethylamine → HCID 13504017, 화합물

HRID 1461133
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HRID 1461133 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

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.

후처리

  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.

출처 및 근거

ORD 기록
ord-8ff175480ca7447dbbd553bfde879b3e
출처 데이터셋
uspto-grants-1991_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05073671

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