HRID1276610
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureHeating
- customwas consumed by thin layer chromatography analysis (340 minutes)
- customThe excess phosgene was removed by codistillation with xylene at atmospheric pressure
- distillationThe distillation
- temperatureThe solution was cooled to room temperature