HRID1730073
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
PROCEDURE
实验过程
A solution of 60 g (0.019 mole) of 3-(4-bromophenacyl)-2,3,5,6-tetrahydrothiopyran-4-one, 1.97 g of 3-dimethylaminopropylamine, 20 ml. of ethanol, and one drop of concentrated hydrochloric acid is heated under reflux under nitrogen for 2.5 hours and allowed to stand overnight during which time crystals precipitated. Recrystallization from ethanol gives colorless crystals of 1-(3-dimethylaminopropyl)-2-(4-bromophenyl)-1,4,6,7-tetrahydrothiopyrano[4,3-b]-pyrrole, m.p. 88° to 90°C.
WORKUP
后处理
- temperatureunder reflux under nitrogen for 2.5 hours
- customprecipitated
- customRecrystallization from ethanol