HRID902320

反应详情

EQUATION

反应方程式

HRID 902320 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 2′,6′-dichloro-5-fluoro-2-methoxybiphenyl (12.44 g, 46 mmol) in methylene chloride (200 mL) was added boron tribromide (10.8 mL, 92 mol) at −78° C. The resulting mixture was stirred at −78° C. to room temperature overnight. The reaction mixture was poured into the ice-NH4OH and extracted with methylene chloride. The organic layer was washed with water and dried over anhydrous sodium sulfate and filtered. The solvent was removed under vacuum. Chromatography with 10–40% ethyl acetate in hexanes afforded 11.63 g (98%) of 2′,6′-dichloro-5-fluorobiphenyl-2-ol as a colorless oil. MS (ES) m/z 255.1([M−H]−).

WORKUP

后处理

  1. extractionextracted with methylene chloride
  2. washThe organic layer was washed with water
  3. dry with materialdried over anhydrous sodium sulfate
  4. filtrationfiltered
  5. customThe solvent was removed under vacuum