HRID62892

反应详情

EQUATION

反应方程式

HRID 62892 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-(4-Methoxy-2,3-dimethyl-phenyl)-cyclopropane carboxylic acid ethyl ester (0.32 g, 1.29 mmol) obtained in Step B was dissolved in DCM (5 mL), and the reactant was cooled to 0˜5° C. BBr3 solution (3.90 mL, 3.87 mmol, 1M/DCM) was added dropwise thereto, and the mixture was stirred at 0˜5° C. for 2 hours. After the termination of the reaction, EtOH and saturated sodium bicarbonate solution were added thereto in turn, and the mixture was stirred. The separated organic layer was concentrated under reduced pressure, and the residue was purified by column chromatography (eluent, EtOAc/Hex=1/5) to obtain the title compound (0.24 g, 79%).

WORKUP

后处理

  1. temperaturethe reactant was cooled to 0˜5° C
  2. additionwere added
  3. stirringin turn, and the mixture was stirred
  4. concentrationThe separated organic layer was concentrated under reduced pressure
  5. customthe residue was purified by column chromatography (eluent, EtOAc/Hex=1/5)