HRID1276610

反应详情

EQUATION

反应方程式

HRID 1276610 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
87.5 °C

PROCEDURE

实验过程

2,3-Dihydro-6-iodo-3-propyl-2-thioxo4(1H)-quinazolinone (50 g, 0.144 mol) was slurried in xylene (283 g) and heated to 85-90° C. Phosgene (12.0 mL, 0.159 mol) was added. Heating was continued until the thioquinazolinedione was consumed by thin layer chromatography analysis (340 minutes). The excess phosgene was removed by codistillation with xylene at atmospheric pressure. The distillation was ceased when the distillate weight reached 37.9 g. The solution was cooled to room temperature and used directly in Step 3.

WORKUP

后处理

  1. temperatureHeating
  2. customwas consumed by thin layer chromatography analysis (340 minutes)
  3. customThe excess phosgene was removed by codistillation with xylene at atmospheric pressure
  4. distillationThe distillation
  5. temperatureThe solution was cooled to room temperature