HRID449176
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
- 52 °C
PROCEDURE
实验过程
The obtained oily product was dissolved in 12 mL acetone to obtain a mixture, then 2 mL water were added to the mixture. Then, a solution of 1.1 mL concentrated sulfuric acid in 3 mL acetone was added dropwise under 10˜15° C. in about 20 min. Then, the mixture was heated to 52° C. and stirred for 1 h. The mixture was cooled by ice water bath under stirring for crystallization. After about 3.5 h later, lots of solid was precipitated. The solid obtained was filtered and dried at 50° C. under vacuum to obtain 5.5 g targeted compound. Yield: 84%, (Calculation by dronedarone hydrochloride), Purity of HPLC: 99.85%.
WORKUP
后处理
- customto obtain a mixture
- temperatureThe mixture was cooled by ice water bath
- stirringunder stirring for crystallization
- waitAfter about 3.5 h later
- customlots of solid was precipitated
- customThe solid obtained
- filtrationwas filtered
- customdried at 50° C. under vacuum
- customto obtain 5.5 g