反应详情

Combine 1-(3,4,5-trimethoxybenzoyl)-3-(2-(4-(1H-benzimidazol-2-yl-amino)piperidin-1-yl)ethyl)-3-phenylpyrrolidine (prepared from (−)-3-phenyl-3-(2-hydroxyethyl)pyrrolidine (R,R)-di-p-anisoyltartaric acid salt) (0.95 g, 1.62 mmol) and ethyl acetate (75 mL). Add a solution of methanesulfonic acid (0.80 g, 8.33 mmol) in ethyl acetate (4 mL). After 18 hours, decant the solvent. Add diethyl ether and stir. After 1 hour, decant, add diethyl ether and stir. After another hour, decant, collect the solid. Combine the solid and methanol and evaporate in vacuo to give a solid. dry in vacuo at 82° C. to give the title compound: mp; 91-104° C. [α]2D0=+1.3° (0.98, methanol).

1. customdecant the solvent
2. waitAfter 1 hour
3. customdecant
4. additionadd diethyl ether
5. stirringstir
6. waitAfter another hour
7. customdecant
8. customcollect the solid
9. customevaporate in vacuo
10. customto give a solid
11. customdry in vacuo at 82° C.