HRID1978965

反应详情

EQUATION

反应方程式

HRID 1978965 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

N-(4-Chlorobenzyl)-4-hydroxy-2-(4-morpholinylmethyl)thieno[2,3-b]pyridine-5-carboxamide (418 mg) from Example No. 41 and potassium carbonate (152 mg) are suspended in DMF (10 mL) and to the mixture is added 1-iodopropane (107 μL). The reaction mixture is allowed to stir at room temperature for 4 h. Additional 1-iodopropane (107 μL) is added and the mixture is heated to 60° C. for 2 h. The mixture is allowed to cool to room temperature and stand for 18 h. The resulting suspension is poured into water (25 mL), filtered, and washed with water (5 mL) followed by diethyl ether (5 mL). The resulting crude solid is purified by recrystallization from ethanol to afford 335 mg (73%) of the title compound as a white solid.

WORKUP

后处理

  1. temperaturethe mixture is heated to 60° C. for 2 h
  2. temperatureto cool to room temperature
  3. waitstand for 18 h
  4. filtrationfiltered
  5. washwashed with water (5 mL)
  6. customThe resulting crude solid is purified by recrystallization from ethanol