HRID50541

反应详情

EQUATION

反应方程式

HRID 50541 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
170 °C

PROCEDURE

实验过程

A solution of 2-chloro-4-phenylamino-quinazoline (0.92 g) (prepared as described in Example 1a and N-methyl-(4-aminophenyl)-methanesulfonamide (0.80 g) in 10 ml of isopentylalcohol is stirred under nitrogen at 170° C. for 15 min in a sealed vessel. The warm reaction mixture is diluted with 10 ml ethanol and the hydrochloride salt, which is crystallizing on cooling, is filtered off to yield N-methyl-[4-(4-phenylamino-quinazolin-2-ylamino)-phenyl]-methanesulfonamide hydrochloride as light yellow crystals melting at 259-263° C.; Rf (A2) 0.11, FAB-MS: (M+H)+=420. Analytical data: C22H21N5O2S+HCl.

WORKUP

后处理

  1. customThe warm reaction mixture
  2. customthe hydrochloride salt, which is crystallizing
  3. temperatureon cooling
  4. filtrationis filtered off