HRID323212
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
Combine 1-(3,4,5-trimethoxybenzoyl)-3-(2-(4-(1-(4-fluorobenzyl)-1H-benzimidazol-2-yl-amino)piperidin-1-yl)ethyl)-3-phenylpyrrolidine (0.45 g) and ethyl acetate (35 mL). Add dropwise a solution of methanesulfonic acid (0.24 g, 2.6 mmol) in ethyl acetate (2.5 mL). After 18 hours, add diethyl ether (100 mL) to form a solid. Repeatedly, decant solvent and add diethyl ether. Again, decant solvent, add diethyl ether, and evaporate in vacuo to give a solid. Dry the solid in vacuo at 82° C. to give the title compound: mp; 131-136° C.
WORKUP
后处理
- customto form a solid
- customRepeatedly, decant solvent
- additionadd diethyl ether
- customAgain, decant solvent
- additionadd diethyl ether
- customevaporate in vacuo
- customto give a solid
- customDry the solid in vacuo at 82° C.