HRID634121

反应详情

EQUATION

反应方程式

HRID 634121 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 2-(1H-indol-5-yl)-5-(methylthio)-1,3,4-thiadiazole (18.5 g, 74.8 mmol) in DMF (190 mL) was added KOH (16.2 g, 299 mmol) followed by I2 (38 g, 149.7 mmol). The reaction was stirred at RT for 2 h, and was quenched with 10% aq sodium bisulphate solution. The resulting precipitate was filtered and washed with H2O to give 2-(3-iodo-1H-indol-5-yl)-5-(methylthio)-1,3,4-thiadiazole (21 g, 75%). MS (ESI, pos. ion) m/z: 373.8 (M+1). 1HNMR (DMSO-d6, 300 MHz): 2.8 (s, 3H), 7.5 (d, 1H), 7.7 (m, 2H), 12.0 (s, 1H).

WORKUP

后处理

  1. customwas quenched with 10% aq sodium bisulphate solution
  2. filtrationThe resulting precipitate was filtered
  3. washwashed with H2O