HRID345045

反应详情

EQUATION

反应方程式

HRID 345045 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Thionyl chloride (1.0.ml) was added dropwise to a stirred mixture of 5-nitrobenzo[b]thiophene-2-methanol (1.0 g) and pyridine (2 drops) in dichloromethane (10 ml). The solution was stirred at room temperature for 4 hours and then washed with water followed by aqueous sodium bicarbonate solution, and then dried (Na2SO4). The solvent was evaporated and the residue was chromatographed on silica gel. Elution with dichloromethane gave a solid which was crystallised from ethyl acetate to give the title compound (0.73 g), m.p. 110°-112°, used directly in the next stage.

WORKUP

后处理

  1. washwashed with water
  2. dry with materialdried (Na2SO4)
  3. customThe solvent was evaporated
  4. customthe residue was chromatographed on silica gel
  5. washElution with dichloromethane
  6. customgave a solid which
  7. customwas crystallised from ethyl acetate