Nitromethane → HCID 57550257, 화합물

HRID 548629노트

반응식

HRID 548629 반응식
[CH2:1]([N:8]1[CH2:12][CH2:11][C:10](=[CH:13][C:14]([O:16][CH3:17])=[O:15])[CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.N12CCCN=C1CCCCC2.[N+:29]([CH3:32])([O-:31])=[O:30]>>[CH2:1]([N:8]1[CH2:12][CH2:11][C:10]([CH2:13][C:14]([O:16][CH3:17])=[O:15])([CH2:32][N+:29]([O-:31])=[O:30])[CH2:9]1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

참가 물질

4

반응물 3

HCID 6375NitromethaneHCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 76563139HCID 76563139, 화합물

생성물 1

HCID 57550257HCID 57550257, 화합물수율 100%

실험 절차

A solution of methyl (1-benzylpyrrolidin-3-ylidene)acetate a45 (3 g, 1.2 mmol, 1 eq), 1,8-diazabicyclo[5.4.0]undec-7-ene (DBU, 0.7 g, 4.6 mmol, 3.8 eq) in nitromethane (30 ml) is refluxed for 30 h. The solution is concentrated in vacuum and the resulting oil is purified by chromatography over silicagel (ethyl acetate/hexane 30/70) to afford 3.7 g of methyl [1-benzyl-3-(nitromethyl)pyrrolidin-3-yl]acetate a46 as a black oil.

후처리

  1. concentrationThe solution is concentrated in vacuum
  2. customthe resulting oil is purified by chromatography over silicagel (ethyl acetate/hexane 30/70)

출처 및 근거

ORD 기록
ord-c9ea4f54a17d4b8ab5620e740ec6bea8
출처 데이터셋
uspto-grants-2011_05
특허 번호
US07943605B2

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