反应详情

Combine 1-(3,4,5-trimethoxybenzoyl)-3-(pyrid-2-yl)-3-(2-oxoethyl)pyrrolidine (0.29 g, 0.75 mmol) and 4-(1-(2-ethoxyethyl)-1H-benzimidazol-2-yl)[1,4]diazepane (0.26 g, 0.91 mmol) silica gel (about 2 g) and 3 Å molecular sieves (about 2 g) in methanol (16 mL). After 18 hours, add sodium cyanoborohydride (0.47 g, 7.5 mmol) and stir. After 7 days, add a solution of 2 M sodium hydroxide and dichloromethane. After 1 hour, filter, separate the layers in the filtrate, dry the organic layer over Na2SO4, filter, and evaporate in vacuo to give a residue. Chromatograph the residue on silica gel eluting with 1/1 methanol/ethyl acetate to give the title compound: mp; 40-42° C. Elemental Analysis calculated for C37H48N6O5.0.75 H2O: C 66.30; H 7.44; N 12.54; Found: C 66.33; H 7.50; N 12.49.

1. waitAfter 7 days
2. waitAfter 1 hour
3. filtrationfilter
4. customseparate the layers in the filtrate
5. dry with materialdry the organic layer over Na2SO4
6. filtrationfilter
7. customevaporate in vacuo
8. customto give a residue