反应详情

Combine 1-(3,4,5-trimethoxybenzoyl)-3-(2-(4-(1-(2-ethoxyethyl)-1H-benzimidazol-2-yl-amino)piperidin-1-yl)ethyl)-3-(3,4-dimethoxyphenyl)pyrrolidine (0.48 g, 0.67 mmol) and ethyl acetate. Add a solution of methanesulfonic acid (2.2 mL, 0.77 M in ethyl acetate, 1.7 mmol). After 24 hours, add diethyl ether (150 mL) to form a solid. Decant solvent, add diethyl ether (200 mL) and stir. After 5 hours, decant solvent, add diethyl ether (200 mL). After 24 hours, collect the solid by filtration and dry in vacuo to give the title compound: mp; 125-130° C. Elemental Analysis calculated for C40H53N5O7 . 2 CH3SO3H . 2.43 H2O: C 53.00; H 6.97; N 7.36; Found: C 53.38; H 6.65; N 7.39.

1. customto form a solid
2. waitAfter 5 hours
3. customdecant solvent
4. additionadd diethyl ether (200 mL)
5. waitAfter 24 hours
6. customcollect the solid
7. filtrationby filtration
8. customdry in vacuo