HRID1362864

反应详情

EQUATION

反应方程式

HRID 1362864 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-[(2-Chloro-5-methyl-4-pyrimidinyl)amino]-N-(1-methylethyl)benzamide (103 mg, 0.337 mmol) and 1-(3-aminophenyl)-4-methyl-2-piperazinone (68.8 mg, 0.335 mmol) were stirred at 95° C. overnight in isopropanol (10 mL) with 12 N HCl (0.056 mL, 0.673 mmol). The reaction was cooled to room temperature and the solid was filtered off and washed with isopropanol. The solid was chromatographed using reverse phase HPLC eluting with 5-30% acetonitrile containing 0.1% formic acid to give a white solid (43 mg, 27%) after lyophilization of the combined HPLC fractions. MS: M(C26H31N7O2)=473.57, (M+H)+=473.8.

WORKUP

后处理

  1. filtrationthe solid was filtered off
  2. washwashed with isopropanol
  3. customThe solid was chromatographed
  4. washeluting with 5-30% acetonitrile containing 0.1% formic acid