HRID442337

反应详情

EQUATION

反应方程式

HRID 442337 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Acetyl chloride (0.6 ml.) was added to a stirred solution of ethyl 6-amino-4-hydroxycinnolin-3-yl carboxylate (0.932 g.) in dry pyridine (20 ml.). The solution was stirred at room temperature for 16 hours and then was poured onto a mixture of ice (100 g.) and 5N-hydrochloric acid (50 ml.). The mixture was kept at 4° C. for 4 hours, and the solid precipitate was then filtered off, washed with water (10 ml.), dried as much as possible on the filter, and recrystallised from ethanol to give ethyl 6-acetylamino-4-hydroxycinnolin-3-yl carboxylate, m.p. 280°-281° C.

WORKUP

后处理

  1. waitThe mixture was kept at 4° C. for 4 hours
  2. filtrationthe solid precipitate was then filtered off
  3. washwashed with water (10 ml.)
  4. customdried as much as possible on the filter
  5. customrecrystallised from ethanol