HRID1466771

反应详情

EQUATION

反应方程式

HRID 1466771 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3-(2-Oxo-propylsulfanyl)-benzoic acid methyl ester (3.65 g, 16.29 mmol) and 3-bromophenylhydrazine hydrochloride (4.01 g, 17.92 mmol) were mixed together in t-BuOH (100 mL) and heated to reflux for 1 hour. After cooling the reaction was concentrated then submitted to standard workup procedure and the crude mixture was purified by silica gel chromatography (0-30% EtOAc in hexanes) to afford a separable 5:4 mixture of regioisomers wherein the title compound was the major product.

WORKUP

后处理

  1. temperatureheated
  2. temperatureto reflux for 1 hour
  3. temperatureAfter cooling the reaction
  4. concentrationwas concentrated
  5. customthe crude mixture was purified by silica gel chromatography (0-30% EtOAc in hexanes)
  6. customto afford