HRID364181

反应详情

EQUATION

反应方程式

HRID 364181 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 20.0 g of 1-chloro-6-methoxy-4-nitro-9H-xanthen-9-one and 27.04 g of anhydrous powdered aluminum chloride was heated under reflux in 400 ml of 1,2-dichloroethane under an argon atmosphere for three hours. The liquid portion of the reaction mixture was decanted and evaporated to a dark residue. Both residues were combined and treated with 200 ml of concentrated hydrochloric acid for one hour. The solid was collected and washed with water and 2-propanol. The grey solid was dried in vacuo at room temperature to afford the title compound, mp 179°-182° C.

WORKUP

后处理

  1. temperaturewas heated
  2. customThe liquid portion of the reaction mixture was decanted
  3. customevaporated to a dark residue
  4. additiontreated with 200 ml of concentrated hydrochloric acid for one hour
  5. customThe solid was collected
  6. washwashed with water and 2-propanol
  7. customThe grey solid was dried in vacuo at room temperature