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 chloroform (3 ml) solution of t-butyl 4-[2-(4-{4-[6-(3,4-dimethoxyphenyl)pyridine-2-carbonyl]piperazin-1-yl}phenoxy)ethyl]piperazine-1-carboxylate was added 0.427 ml of a 4M hydrogen chloride/ethyl acetate solution, followed by 2 days of stirring at room temperature. Further, 2 ml of chloroform and 1 ml of a 4M hydrogen chloride/ethyl acetate solution were added thereto, and the whole was stirred at room temperature overnight. Ethanol was added to the reaction mixture and crude crystals were collected by filtration and recrystallized from methanol to obtain 114 mg of 1-[6-(3,4-dimethoxyphenyl)pyridine-2-carbonyl]-4-[4-(2-piperazin-1-ylethoxy)phenyl]piperazine tetrahydrochloride hydrate as pale yellow crystals.
WORKUP
后处理
- stirringthe whole was stirred at room temperature overnight
- filtrationcrude crystals were collected by filtration
- customrecrystallized from methanol