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

HRID 1504330ノート

反応式

HRID 1504330 の反応式
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

参加物

5

反応物 3

HCID 962WaterHCID 3939Lithium HydroxideHCID 86682803HCID 86682803、化合物

生成物 1

HCID 866828054-Bromo-2-chloro-5-trifluoromethoxy-benzoic acid収率 100.8%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
60 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-09a9b6bceccd46d68439d05de89c2d39
出典データセット
uspto-grants-2015_12
特許番号
US09212168B2

反応ノート

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