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

HRID 1857624노트

반응식

HRID 1857624 반응식
[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]

참가 물질

3

반응물 2

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

생성물 1

HCID 15895692Methyl 2-amino-4-chloro-5-nitrobenzoate수율 95%

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-91e5a302a6c846f68d59165c6c407441
출처 데이터셋
uspto-grants-2000_11
특허 번호
US06147088

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