HRID1452055

反应详情

EQUATION

反应方程式

HRID 1452055 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

5,7-Dichloro-4-[4-(methylcarbamoyl)-3-chlorobenzenesulfonimide]-1,4-dihydroquinoline-2-carboxylic acid, methyl ester ##STR38## Dissolve 4-amino-3-chlorobenzenesulfonamide (0.96g, 5mmol) in chlorobenzene (10% solution) and distill the mixture to remove any traces of water. Cool to 100° C. and add n-butyl isocyanate (99mg, 1mmol). Heat to reflux and add, by dropwise addition, oxalyl chloride (1.5mL). Purge with nitrogen at 130°-132° C. for 30 minutes and distill to give 3-chloro-4-isocyanatobenzenesulfonyl isocyanate.

WORKUP

后处理

  1. distillationdistill the mixture
  2. customto remove any traces of water
  3. temperatureHeat
  4. temperatureto reflux
  5. customPurge with nitrogen at 130°-132° C. for 30 minutes
  6. distillationdistill