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
To a solution of N-[4-[N-methyl-N-(tetrahydropyran-4-yl)aminomethyl]phenyl]-7-(4-morpholinophenyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxamide (36 mg) in ethanol/methanol (10/5 ml) was added at room temperature concentrated hydrochloric acid (0.5 ml), and the mixture was stirred for a few minutes. Insoluble materials were filtered off, and the filtrate was concentrated under reduced pressure. To the residue was added diethylether, and precipitated solid was collected by filtration, which was washed with diethylether to give yellow powder of N-[4-[N-methyl-N-(tetrahydropyran-4-yl)aminomethyl]phenyl]-7-(4-morpholinophenyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxamide dihydrochloride (Compound 2) (34 mg).
WORKUP
后处理
- filtrationInsoluble materials were filtered off
- concentrationthe filtrate was concentrated under reduced pressure
- additionTo the residue was added diethylether
- customprecipitated solid
- filtrationwas collected by filtration, which
- washwas washed with diethylether