HRID1978935

反应详情

EQUATION

反应方程式

HRID 1978935 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-iodothieno[2,3-b]pyridine-5-carboxamide (Example No. 2) (0.500 g) in pyridine (5 mL) is added CuCN (0.201 g). The reaction is heated to reflux and stirred for 18 h. The reaction mixture is purified via column chromatography (CH2Cl2:CH3OH; 98:2). Fractions homogeneous by TLC are combined and concentrated in vacuo to yield a pale yellow solid which is recrystallized from methanol to yield 0.100 g (26%) of the title compound as an off-white solid.

WORKUP

后处理

  1. temperatureThe reaction is heated
  2. temperatureto reflux
  3. customThe reaction mixture is purified via column chromatography (CH2Cl2:CH3OH; 98:2)
  4. concentrationconcentrated in vacuo
  5. customto yield a pale yellow solid which
  6. customis recrystallized from methanol