Benzoic acid, 3-methyl-2-nitro-, methyl ester → Methyl 2-nitro-3-(2-oxo-n-propyl)benzoate

HRID 274573

반응식

HRID 274573 반응식
[CH3:1][C:2]1[C:3]([N+:12]([O-:14])=[O:13])=[C:4]([CH:9]=[CH:10][CH:11]=1)[C:5]([O:7][CH3:8])=[O:6].C[O:16][C:17](OC)(N(C)C)[CH3:18]>CC(N(C)C)=O>[N+:12]([C:3]1[C:2]([CH2:1][C:17](=[O:16])[CH3:18])=[CH:11][CH:10]=[CH:9][C:4]=1[C:5]([O:7][CH3:8])=[O:6])([O-:14])=[O:13]

참가 물질

4

반응물 2

HCID 79621Benzoic acid, 3-methyl-2-nitro-, methyl esterHCID 878351,1-Dimethoxyethyl(dimethyl)amine

생성물 1

HCID 20093000Methyl 2-nitro-3-(2-oxo-n-propyl)benzoate수율 23%

시약·촉매·용매 1

HCID 31374Dimethylacetamide용매

실험 절차

A solution of methyl 3-methyl-2-nitrobenzoate (1.5 g) and N,N-dimethylacetamide dimethyl acetal (3 ml) in dimethylacetamide (5 ml) was heated at 140° C. for 3 hours. After evaporation of the solvent, the resulting brown syrup was dissolved in ethyl acetate. The solution was washed with water, dried and concentrated to dryness. The residue was purified by column chromatography on silica gel to give a pale brown syrup (0.42 g, 23%).

후처리

  1. customAfter evaporation of the solvent
  2. dissolutionthe resulting brown syrup was dissolved in ethyl acetate
  3. washThe solution was washed with water
  4. customdried
  5. concentrationconcentrated to dryness
  6. customThe residue was purified by column chromatography on silica gel

출처 및 근거

ORD 기록
ord-fe9bd6788f2f482bad06ce005701ad2a
출처 데이터셋
uspto-grants-1995_02
특허 번호
US05389641

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