Nitromethane → Benzenepropanoic acid, b-(nitromethyl)-, methyl ester

HRID 1045677

반응식

HRID 1045677 반응식
[C:1]([O:11][CH3:12])(=[O:10])[CH:2]=[CH:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.[N+:13]([CH3:16])([O-:15])=[O:14]>>[CH3:12][O:11][C:1](=[O:10])[CH2:2][CH:3]([C:4]1[CH:5]=[CH:6][CH:7]=[CH:8][CH:9]=1)[CH2:16][N+:13]([O-:15])=[O:14]

참가 물질

3

반응물 2

HCID 6375NitromethaneHCID 76442-Propenoic acid, 3-phenyl-, methyl ester

생성물 1

HCID 10537045Benzenepropanoic acid, b-(nitromethyl)-, methyl ester수율 59%

실험 절차

A solution of methyl cinnamate (4.93 g, 30.4 mmol) and teteramethylguanidine (3.99 g, 34.6 mmol) in nitromethane (30 ml) was stirred for 6 hours at 90° C. After removal of the solvent under reduced pressure, the residue was partitioned between water and ethyl acetate, and the organic layer was washed with water and brine and then dried over sodium sulfate. The organic solvents were removed under reduced pressure, and the residue was purified by silica gel column chromatography (eluent; hexane/ethyl acetate=4/1) to afford 4-nitro-3-phenyl-butyric acid methyl ester (4.02 g, 59%)

후처리

  1. customAfter removal of the solvent under reduced pressure
  2. customthe residue was partitioned between water and ethyl acetate
  3. washthe organic layer was washed with water and brine
  4. dry with materialdried over sodium sulfate
  5. customThe organic solvents were removed under reduced pressure
  6. customthe residue was purified by silica gel column chromatography (eluent; hexane/ethyl acetate=4/1)

출처 및 근거

ORD 기록
ord-c8e60e5b5cfc4570bdec6bafcfa9603c
출처 데이터셋
uspto-grants-2013_10
특허 번호
US08569294B2

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