HRID515259

反应详情

EQUATION

反应方程式

HRID 515259 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1-(2-hydroxyethyl)piperazine (Compound 3) (65 g, 0.5 mol), 2-(6-bromo-2-methylpyrimidin-4-ylamino)-N-(2-chloro-6-methylphenyl)thiazole-5-formamide (Compound 14) (43.9 g, 0.1 mol), n-butanol (670 mL) and DIPEA (28.3 g, 0.2 mol) were mixed in reaction flask and reacted by refluxing for 7 h. After the reactant was cooled down to room temperature, crystals precipitated overnight. After air pump filtration, the cake was rinsed with n-butanol (500 mL) by stirring for 30 min. Then filtrated and the cake was dried to give white solid target Compound 1 (42.9 g, yield: 87.9%).

WORKUP

后处理

  1. customreacted
  2. temperatureby refluxing for 7 h
  3. customcrystals precipitated overnight
  4. filtrationAfter air pump filtration
  5. washthe cake was rinsed with n-butanol (500 mL)
  6. filtrationThen filtrated
  7. customthe cake was dried