Methyl 2-methyl-3-nitrobenzoate → 3-Amino-2-methylbenzoic acid methyl ester

HRID 1285

反応式

HRID 1285 の反応式
[CH3:1][C:2]1[C:11]([N+:12]([O-])=O)=[CH:10][CH:9]=[CH:8][C:3]=1[C:4]([O:6][CH3:7])=[O:5]>C(O)(=O)C.[Pd]>[CH3:1][C:2]1[C:11]([NH2:12])=[CH:10][CH:9]=[CH:8][C:3]=1[C:4]([O:6][CH3:7])=[O:5]

参加物

4

反応物 1

HCID 601165Methyl 2-methyl-3-nitrobenzoate

生成物 1

HCID 38010253-Amino-2-methylbenzoic acid methyl ester収率 101.6%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 176Acetic Acid溶媒

実験手順

Methyl 2-methyl-3-nitrobenzoate (10.0 g) is dissolved in acetic acid (50 ml) and thereto 5% Pd-C (1 g) is added to carry out catalytic reduction at room temperature under 1 atm. After 1.5 hours, the catalyst is filtered off. The reaction mixture is concentrated, and thereto is added water, and the mixture is made alkaline with potassium carbonate, followed by extraction with dichloromethane. The solvent is concentrated to give methyl 2-methyl-3-aminobenzoate (8.6 g).

後処理

  1. customat room temperature
  2. filtrationthe catalyst is filtered off
  3. concentrationThe reaction mixture is concentrated
  4. additionis added water
  5. extractionfollowed by extraction with dichloromethane
  6. concentrationThe solvent is concentrated

出典と根拠

ORDレコード
ord-a382dee7401645edb9da6c1fce7078a0
出典データセット
uspto-grants-1998_03
特許番号
US05723648

関連ノート

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