HRID326437
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
- 20 °C
PROCEDURE
实验过程
Hydroiodic acid (50%, 205 parts) was added to 2-(3-methoxyphenyl)-1,3-indandione (67.1 parts) and the mixture was stirred under reflux for 10 minutes. By-product methyl iodide was removed by distillation and the solution was cooled to 20° C. The aqueous layer was decanted to leave a red oil. The oil was dissolved in chloroform (250 parts), washed with water (100 parts), separated and dried over anhydrous magnesium sulphate. The chloroform was removed by evaporation under reduced pressure to leave an orange solid. The solid was crystallised from toluene (1800 parts) to yield 2-(3-hydroxyphenyl)-1,3-indandione (30.6 parts), m.pt. 139°-141° C.
WORKUP
后处理
- temperatureunder reflux for 10 minutes
- customBy-product methyl iodide was removed by distillation
- customThe aqueous layer was decanted
- customto leave a red oil
- washwashed with water (100 parts)
- customseparated
- dry with materialdried over anhydrous magnesium sulphate
- customThe chloroform was removed by evaporation under reduced pressure
- customto leave an orange solid
- customThe solid was crystallised from toluene (1800 parts)