Hydrochloric Acid → 6-Bromo-3-(difluoromethoxy)-2-methoxyphenol

HRID 2171092ノート

反応式

HRID 2171092 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH:9]([F:11])[F:10])=[C:4]([O:12][CH3:13])[C:3]=1[O:14]COC.Cl>CO>[Br:1][C:2]1[C:3]([OH:14])=[C:4]([O:12][CH3:13])[C:5]([O:8][CH:9]([F:10])[F:11])=[CH:6][CH:7]=1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 674667461-Bromo-4-(difluoromethoxy)-3-methoxy-2-(methoxymethoxy)benzene

生成物 1

HCID 674670406-Bromo-3-(difluoromethoxy)-2-methoxyphenol収率 93.2%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
50 °C

実験手順

To a stirring solution of 1-bromo-4-(difluoromethoxy)-3-methoxy-2-(methoxymethoxy)benzene (1 g, 3.19 mmol) in methanol (15 mL) was added concentrated hydrochloride (2 mL) and the reaction mixture was heated to 50° C. for 1 h. The reaction mixture was cooled to RT, concentrated under reduced pressure and the obtained residue was basified with sodium bicarbonate solution and extracted with dichloromethane (3×). The combined dichloromethane layers were washed with brine, dried over sodium sulphate and concentrated under reduced pressure to afford the title compound as a solid (800 mg, 93%).

後処理

  1. temperatureThe reaction mixture was cooled to RT
  2. concentrationconcentrated under reduced pressure
  3. extractionextracted with dichloromethane (3×)
  4. washThe combined dichloromethane layers were washed with brine
  5. dry with materialdried over sodium sulphate
  6. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-52dc51a924b54c9d8c3c20a2acf80d1c
出典データセット
uspto-grants-2015_06
特許番号
US09051290B2

反応ノート

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