HRID2366212

反应详情

EQUATION

反应方程式

HRID 2366212 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

Trimethylsilylbromide (0.23 mL, 1.74 mmol) was added to a stirred solution of 3,5-dichloro-4-(4-chloro-thiazolo[5,4-c]pyridine-2-yl)-benzonitrile (295 mg, 0.87 mmol) in propionitrile (11 mL) and the mixture heated at 90° C. for 48 hours. The reaction mixture was allowed to cool and poured onto a mixture of saturated aqueous potassium carbonate solution and ice. DCM was added and the organic phase was separated, dried over Na2SO4 and concentrated to dryness under reduced pressure to give the desired compound as a white solid (322 mg, 96% yield). 1H NMR (300 MHz, CDCl3): δ 8.53 (d, J=5.5 Hz, 1H), 8.03-8.00 (m, 1H), 7.80 (s, 2H). LCMS (Method D): RT=4.04 min, m/z: 386 [M+H+].

WORKUP

后处理

  1. temperatureto cool
  2. customthe organic phase was separated
  3. dry with materialdried over Na2SO4
  4. concentrationconcentrated to dryness under reduced pressure