HRID23623

反应详情

EQUATION

反应方程式

HRID 23623 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

A mixture of N-(4-chlorobenzyl)-7-hydroxy-2-(hydroxymethyl)-3-methylthieno[3,2-b]pyridine-6-carboxamide (100 mg, 0.276 mmol), potassium carbonate (57 mg, 0.41 mmol) and iodoacetamide (255 mg, 1.38 mmol) in DMF (1.5 mL) was stirred at 50° C. for 18 hrs. Additional iodoacetamide (255 mg) and potassium carbonate (57 mg) were added, and the reaction was stirred at the same temperature for another 12 hrs. After cooling, cold water was added, and the resulting ppt was collected by filtration after chilling in an ice bath. The collected crude solid was recrystallized from aq. ethanol to give the title compound (65 mg) as a lt. brown solid.

WORKUP

后处理

  1. stirringthe reaction was stirred at the same temperature for another 12 hrs
  2. temperatureAfter cooling
  3. filtrationthe resulting ppt was collected by filtration
  4. temperatureafter chilling in an ice bath
  5. customThe collected crude solid
  6. customwas recrystallized from aq. ethanol