HRID623716

反应详情

EQUATION

反应方程式

HRID 623716 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

A mixture of 3,3′-thiodipropanoic acid (1 equivalent) and thiosemicarbazide (2 equivalents) were taken in POCl3 (10 fold) and stirred at 90° C. for 3 h. The reaction mixture was cooled to room temperature and poured on to ice. The resulting mixture was filtered and then brought to pH 14 using KOH. The white solid that was formed was filtered, washed with water and dried to afford the desired product I-2 in 50-60% yield. This material was used as such for the next step.

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled to room temperature
  2. additionpoured on to ice
  3. filtrationThe resulting mixture was filtered
  4. customThe white solid that was formed
  5. filtrationwas filtered
  6. washwashed with water
  7. customdried