HRID1700380
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
3.8 g of the compound obtained in Step C are stirred for 72 hours at ambient temperature in 200 ml of tetrahydrofuran and 10 ml of a 1 M solution of tetrabutylammonium fluoride in tetrahydrofuran in the presence of 1 g of 3 Å molecular sieve. After filtering off the resin and evaporating to dryness, the residue is taken up in 100 ml of 1N HCl and washed with dichloromethane. The aqueous phase is then rendered alkaline and extracted with dichloromethane and the combined organic phases are worked up in customary manner. The product obtained crystallises as the hydrochloride in an ethanol-diethyl ether-hydrogen chloride mixture.
WORKUP
后处理
- filtrationAfter filtering off the resin
- customevaporating to dryness
- washwashed with dichloromethane
- extractionextracted with dichloromethane
- customThe product obtained
- customcrystallises as the hydrochloride in an ethanol-diethyl ether-hydrogen chloride mixture