HRID573617

反应详情

EQUATION

反应方程式

HRID 573617 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of N-{2-bromo-6-methyl-3-[3-(methyloxy)phenyl]thieno[2,3-b]pyridin-4-yl}-3-chlorobenzenesulfonamide (85 mg, 0.162 mmol) (Example 33), potassium ferrocyanide (13.71 mg, 0.032 mmol), copper(I) iodide (3.09 mg, 0.016 mmol) in 1-methylimidazole (1 mL, 12.55 mmol) was subjected to microwave reaction at 160° C. for 1 h. Purification by chromatography on silica gel, eluting with a gradient of 40-60% ethyl acetate in cyclohexane, afforded the title compound (24 mg). LCMS (A) m/z: 470 [M+1]+, Rt 1.58 min (acidic), Rt 1.09 min (basic).

WORKUP

后处理

  1. customreaction at 160° C. for 1 h
  2. customPurification by chromatography on silica gel
  3. washeluting with a gradient of 40-60% ethyl acetate in cyclohexane