HRID1978957

反应详情

EQUATION

反应方程式

HRID 1978957 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of N-(4-chlorobenzyl)-4-hydroxy-2-(hydroxymethyl)thieno[2,3-b]pyridine-5-carboxamide (0.955 g) from Example No. 34 in DMF (20 mL) is added potassium carbonate (0.567 g) followed by iodomethane (0.20 mL). The reaction is stirred at rt for 1 h. The reaction mixture is partitioned between water (50 mL) and CH2Cl2 (100 mL). The aqueous layer is extracted with CH2Cl2 (100 mL). The organic layer is removed in vacuo and insoluble material in the aqueous layer is filtered off. The resulting solid is recrystallized from ethanol to yield 0.825 g (83%) of the title compound as a white, crystalline solid.

WORKUP

后处理

  1. customThe reaction mixture is partitioned between water (50 mL) and CH2Cl2 (100 mL)
  2. extractionThe aqueous layer is extracted with CH2Cl2 (100 mL)
  3. customThe organic layer is removed in vacuo and insoluble material in the aqueous layer
  4. filtrationis filtered off
  5. customThe resulting solid is recrystallized from ethanol