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

HRID 274573

反応式

HRID 274573 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 31374Dimethylacetamide溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-fe9bd6788f2f482bad06ce005701ad2a
出典データセット
uspto-grants-1995_02
特許番号
US05389641

関連ノート

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