1-(2-Amino-3-chloro-4-methoxyphenyl)ethanone → 1-(2-Amino-3-chloro-4-hydroxy-phenyl)-ethanone

HRID 2405844노트

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HRID 2405844 반응식
[NH2:1][C:2]1[C:7]([Cl:8])=[C:6]([O:9]C)[CH:5]=[CH:4][C:3]=1[C:11](=[O:13])[CH3:12]>Br>[NH2:1][C:2]1[C:7]([Cl:8])=[C:6]([OH:9])[CH:5]=[CH:4][C:3]=1[C:11](=[O:13])[CH3:12]

참가 물질

3

반응물 1

HCID 299199881-(2-Amino-3-chloro-4-methoxyphenyl)ethanone

생성물 1

HCID 574451951-(2-Amino-3-chloro-4-hydroxy-phenyl)-ethanone수율 61%

시약·촉매·용매 1

HCID 260Hydrogen Bromide용매

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온도
0 °C

실험 절차

1-(2-Amino-3-chloro-4-methoxyphenyl)ethanone (prepared according to Raboisson, P. J.-M. B., et al., WO2007014926, p 78; 70.7 g, 354 mmol) was stirred in 48% aq. HBr (500 mL) at 110° C. for 72 h. After the mixture was cooled to 0° C. with stirring, the solids were filtered and washed with water. The resulting solids were triturated with a saturated NaHCO3 solution (˜350 mL), filtered, washed with water, and dried under vacuum to give 40 g (61% yield) of 1-(2-amino-3-chloro-4-hydroxyphenyl)ethanone as a dark brown solid.

후처리

  1. filtrationthe solids were filtered
  2. washwashed with water
  3. customThe resulting solids were triturated with a saturated NaHCO3 solution (˜350 mL)
  4. filtrationfiltered
  5. washwashed with water
  6. customdried under vacuum

출처 및 근거

ORD 기록
ord-126b56a0e34443a7804b441765632678
출처 데이터셋
uspto-grants-2014_08
특허 번호
US08809267B2

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