HRID2307294

反应详情

EQUATION

反应方程式

HRID 2307294 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Potassium carbonate (0.91 g) and 1-iodopropane (0.64 mL) are added to a solution of N-(4-chlorobenzyl)-4-hydroxy-2-(hydroxymethyl)thieno[2,3-b]pyridine-5-carboxamide (2.0 g, prepared as described in U.S. Pat. No. 6,239,142) in anhydrous DMF (60 mL). The reaction mixture is stirred at room temperature for 4 h. The mixture is diluted with water (150 mL) and filtered. The resulting white powder is washed with water (15 mL) followed by diethyl ether (15 mL) and dried in a vacuum oven to afford 1.73 g of the title compound as a white solid Physical characteristics. Mp 174-175° C. 1H NMR (300 MHz, DMSO-d6) δ 10.62, 8.72, 7.38, 7.29, 5.80, 4.69, 4.55, 4.27, 1.87, 0.89; Anal. Found: C, 58.20; H, 4.96; N. 7.13; Cl, 8.98; S, 8.16.

WORKUP

后处理

  1. customprepared
  2. filtrationfiltered
  3. washThe resulting white powder is washed with water (15 mL)
  4. customdried in a vacuum oven