HRID2386696

反应详情

EQUATION

反应方程式

HRID 2386696 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A solution of 6-[2-(2-chloro-5-methoxy-phenyl)-1-hydroxy-1-trifluoromethyl-propyl]-4-methyl-4H-benzo[1,4]oxazin-3-one (553 mg) in dichloromethane (13 ml) was cooled to −70° C. A 1 M solution of boron tribromide in dichloromethane (5.14 ml) was added and the mixture was stirred at −70° C. for 1.5 h and at 0° C. for 1 h. A mixture of ice water and saturated aqueous NaHCO3 solution was added and the mixture was extracted with dichloromethane. The organic phase was washed with water and dried (MgSO4). The product was purified by chromatography (SiO2, cyclohexane/EtOAc 9:1=>2:3) to give the title compound (542 mg) as off-white foam. MS (m/e, ISP neg. ion)=414.0 [M−H+].

WORKUP

后处理

  1. additionwas added
  2. extractionthe mixture was extracted with dichloromethane
  3. washThe organic phase was washed with water
  4. dry with materialdried (MgSO4)
  5. customThe product was purified by chromatography (SiO2, cyclohexane/EtOAc 9:1=>2:3)