HRID66345

反应详情

EQUATION

反应方程式

HRID 66345 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

n-Butyl isocyanate (11.2 cc.) is added over the course of 15 minutes to a suspension of 5-chloro-2-(7-chloro-1,8-naphthyridin-2-yl)-3-hydroxy-isoindolin-1-one (3.5 g.) in acetonitrile (350 cc.) and triethylamine (0.2 cc.) heated at the reflux temperature. Pyridine (10 cc.) and triethylamine (5 cc.) are added and refluxing is continued for a further 40 minutes. After filtering hot and then cooling, the precipitate formed is filtered off and recrystallised from acetonitrile (250 cc.) to give 5-chloro-2-(7-chloro-1,8-naphthyridin-2-yl)-3-n-butylaminocarbonyloxy-isoindolin-1-one (3.3 g.) melting at 228°-230° C.

WORKUP

后处理

  1. temperatureheated at the reflux temperature
  2. temperaturerefluxing
  3. filtrationAfter filtering hot
  4. temperaturecooling
  5. customthe precipitate formed
  6. filtrationis filtered off
  7. customrecrystallised from acetonitrile (250 cc.)