Sulfuric Acid → Methyl 2-amino-4-chloro-5-nitrobenzoate

HRID 1275594ノート

反応式

HRID 1275594 の反応式
[CH3:1][O:2][C:3](=[O:18])[C:4]1[CH:9]=[C:8]([N+:10]([O-:12])=[O:11])[C:7]([Cl:13])=[CH:6][C:5]=1[NH:14]C(=O)C.S(=O)(=O)(O)O>>[CH3:1][O:2][C:3](=[O:18])[C:4]1[CH:9]=[C:8]([N+:10]([O-:12])=[O:11])[C:7]([Cl:13])=[CH:6][C:5]=1[NH2:14]

参加物

3

反応物 2

HCID 1118Sulfuric AcidHCID 544712152-Acetylamino-4-chloro-5-nitrobenzoic acid methyl ester

生成物 1

HCID 15895692Methyl 2-amino-4-chloro-5-nitrobenzoate収率 95%

実験手順

To a solution of 2-acetylamino-4-chloro-5-nitrobenzoic acid methyl ester (1.02 g in 15 mL methanol) was added 1 mL of conc. sulfuric acid and the mixture heated to reflux on an oil bath. After 1 hour, the mixture was concentrated in vacuo and the resulting solid dissolved in 200 mL ethyl acetate. This was then washed with 10% sodium bicarbonate (2×100 mL) and brine (100 mL) and the organics dried over magnesium sulfate. The concentrate was recrystallized from methanol to give the title compound (0.82 g).

後処理

  1. temperaturethe mixture heated
  2. temperatureto reflux on an oil bath
  3. concentrationthe mixture was concentrated in vacuo
  4. dissolutionthe resulting solid dissolved in 200 mL ethyl acetate
  5. washThis was then washed with 10% sodium bicarbonate (2×100 mL) and brine (100 mL)
  6. dry with materialthe organics dried over magnesium sulfate
  7. customThe concentrate was recrystallized from methanol

出典と根拠

ORDレコード
ord-2de1b14513ac4280ba3d8e149f31e747
出典データセット
uspto-grants-2000_12
特許番号
US06162813

反応ノート

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