Water → 4-Bromo-2-chloro-5-trifluoromethoxy-benzoic acid

HRID 1504330노트

반응식

HRID 1504330 반응식
C[O:2][C:3](=[O:17])[C:4]1[CH:9]=[C:8]([O:10][C:11]([F:14])([F:13])[F:12])[C:7]([Br:15])=[CH:6][C:5]=1[Cl:16].O.[OH-].[Li+]>CO>[Br:15][C:7]1[C:8]([O:10][C:11]([F:12])([F:13])[F:14])=[CH:9][C:4]([C:3]([OH:17])=[O:2])=[C:5]([Cl:16])[CH:6]=1

참가 물질

5

반응물 3

HCID 962WaterHCID 3939Lithium HydroxideHCID 86682803HCID 86682803, 화합물

생성물 1

HCID 866828054-Bromo-2-chloro-5-trifluoromethoxy-benzoic acid수율 100.8%

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
60 °C

실험 절차

To a mixture of 4-bromo-2-chloro-5-trifluoromethoxy-benzoic acid methyl ester (1.0 g, 3.0 mmol, Preparation 48) dissolved in methanol (4 mL) and water (4 mL) was added lithium hydroxide (360 mg, 15 mmol). The reaction mixture was stirred at 60° C. for 1 h and concentrated. The reaction mixture was adjusted to acidic pH with 1 N HCl, dissolved in EtOAc (60 mL) and washed with water (60 mL). The aqueous layer was extracted with EtOAc (60 mL). The combined organic layers were washed with brine, dried over sodium sulfate, filtered, and concentrated to produce the title intermediate (966 mg, 100% yield) as a white powder.

후처리

  1. concentrationconcentrated
  2. dissolutiondissolved in EtOAc (60 mL)
  3. washwashed with water (60 mL)
  4. extractionThe aqueous layer was extracted with EtOAc (60 mL)
  5. washThe combined organic layers were washed with brine
  6. dry with materialdried over sodium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated

출처 및 근거

ORD 기록
ord-09a9b6bceccd46d68439d05de89c2d39
출처 데이터셋
uspto-grants-2015_12
특허 번호
US09212168B2

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