HRID474593

反应详情

EQUATION

反应方程式

HRID 474593 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 4-chloro-3-(trifluoromethyl)phenyl 4-ethenyl-2-fluorophenyl ether (4.0 g, 12.63 mmol) in THF (13 mL) was added dropwise 9-BBN (50.5 mL, 25.3 mmol) at 0° C. The reaction mixture was stirred at room temperature for overnight, then mixed with NaOH (25.3 mL, 76 mmol) and H2O2 (7.74 mL, 76 mmol). The mixture was stirred at 55° C. for 4 h, quenched by Na2SO3, and extracted with EA (100 mL×3). Organic phases were collected, combined, dried with anhydrous Na2SO4, and concentrated to provide the title compound (4.02 g, 95% yield). LCMS: rt=4.6 min, [M+H+]=334

WORKUP

后处理

  1. stirringThe mixture was stirred at 55° C. for 4 h
  2. customquenched by Na2SO3
  3. extractionextracted with EA (100 mL×3)
  4. customOrganic phases were collected
  5. dry with materialdried with anhydrous Na2SO4
  6. concentrationconcentrated