HRID734729

反应详情

EQUATION

反应方程式

HRID 734729 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-78 °C

PROCEDURE

实验过程

BBr3 (4 mL, 4 mmol, 1.0 M in heptane) was added dropwise to a solution of 2-fluoro-5-(methyloxy)benzaldehyde in CH2Cl2 at −78° C. The reaction mixture was stirred at −78° C. for 1 hour, slowly warmed to 0° C. and stirred for 2 hours. The reaction mixture was poured into water, extracted with EtOAc (3×10 mL). The extracts were combined, washed with water, brine, and dried (Na2SO4). The solvent was evaporated, and the residue was purified on silica gel, using 0-20% EtOAc-Hexane to give the desired product (142 mg, 25%) as a white solid. MS m/z 141 [M+H]+

WORKUP

后处理

  1. temperatureslowly warmed to 0° C.
  2. stirringstirred for 2 hours
  3. extractionextracted with EtOAc (3×10 mL)
  4. washwashed with water, brine
  5. dry with materialdried (Na2SO4)
  6. customThe solvent was evaporated
  7. customthe residue was purified on silica gel