反应详情

温度

5 °C

Combine 1-(3,4,5-trimethoxy-benzoyl)-3-[2-[4-[1-(3-ethoxycarbonyl-propyl)-1 H-benzoimidazole-2-carbonyl]-piperidin-1-yl]-ethyl]-3-(3,4-dichloro-phenyl)-pyrrolidine (0.32 g, 0.41 mmol) and lithium hydroxide hydrate (0.052 g, 1.23 mmol) in 4/1 tetrahydrofuran/water (20 mL). After 20 hours, dilute the reaction mixture with water and evaporate in vacuo to remove most of the tetrahydrofuran. Acidify to pH 2 using 1 M hydrochloric acid solution and cool to 5° C. to obtain a solid. Collect the solid by filtration. Suspend the solid in diethyl ether (150 mL) and stir. After 18 hours, collect the solid by filtration and dry to give the title compound: mp; 125-140° C. Elemental Analysis calculated for C39H44Cl2N4O7·HCl: C 59.43; H 5.75; N 7.11; Found: C 59.55; H 5.81; N 6.94.

1. customevaporate in vacuo
2. customto remove most of the tetrahydrofuran
3. customto obtain a solid
4. customCollect the solid
5. filtrationby filtration
6. waitAfter 18 hours
7. customcollect the solid
8. filtrationby filtration
9. customdry