HRID645700

反应详情

EQUATION

反应方程式

HRID 645700 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
115 °C

PROCEDURE

实验过程

To a mixture of N-(1H-benzo[d]imidazol-6-yl)-2-chloro-7-tosyl-7H-pyrrolo[2,3-d]pyrimidin-4-amine (0.1 g, 0.24 mmol) in n-butyl alcohol (1 mL) was added 1-(4-aminophenyl)-N,N-dimethylpiperidine-4-carboxamide (0.11 g, 0.44 mmol) and TMSCl (0.014 mL, 0.11 mmol). After heating at 115° C. for 15 h, the mixture was diluted with MeOH (1 mL), and a solution of KOH (0.1 g) in H2O (0.5 mL) was added. After heating at 60° C. for 2 h, the mixture was purified by preparative HPLC to give 1-(4-(4-(1H-benzo[d]imidazol-6-ylamino)-7H-pyrrolo[2,3-d]pyrimidin-2-ylaminophenyl)-N,N-dimethylpiperidine-4-carboxamide (0.02 g, MS (MH 496.3) (Compound 18-1).

WORKUP

后处理

  1. temperatureAfter heating at 60° C. for 2 h
  2. customthe mixture was purified by preparative HPLC