HRID375081

反应详情

EQUATION

反应方程式

HRID 375081 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A solution of the oxime of 2'-methoxy-2-(methylthio)-5-nitrobenzophenone (8.3 g, 26.1 mmol) and acetic anhydride (20 mL) in pyridine (150 mL) is refluxed for 5 days, cooled and concentrated in vacuo to obtain a dark solid. A mixture of the solid in methanol is acidified with concentrated hydrochloric acid (pH5), diluted with water and filtered to obtain a solid. A solution of the solid in methylene chloride is passed through a silica gel pad and concentrated in vacuo to give the title product as a solid, mp 193°-198° C.

WORKUP

后处理

  1. temperaturecooled
  2. concentrationconcentrated in vacuo
  3. customto obtain a dark solid
  4. filtrationfiltered
  5. customto obtain a solid
  6. concentrationconcentrated in vacuo