反应详情

温度

100 °C

A mixture of ethyl 5,6-dichloronicotinate (5.0 g), tert-butyl (3R)-3-amino-1-pyrrolidinecarboxylate (5.08 g) and K2CO3 (4.71 g) in DMF (40 ml) was stirred at 100° C. for 12 hours under atmospheric pressure of nitrogen. The reaction mixture was poured into a mixture of AcOEt and H2O and the organic layer was washed with brine and dried over MgSO4. The solvent was evaporated in vacuo and the residue was chromatographed on silicagel eluting with n-Hexane-AcOEt (9:1). The eluted fractions containing the desired product were collected and evaporated in vacuo to give ethyl 6-{[(3R)-1-(tert-butoxycarbonyl)-3-pyrrolidinyl]amino}-5-chloronicotinate (6.6 g).

1. washthe organic layer was washed with brine
2. dry with materialdried over MgSO4
3. customThe solvent was evaporated in vacuo
4. customthe residue was chromatographed on silicagel
5. washeluting with n-Hexane-AcOEt (9:1)
6. additionThe eluted fractions containing the desired product
7. customwere collected
8. customevaporated in vacuo