反应详情

A solution of 1-amino-3-{[4-(2,3-dichlorophenyl)-3-ethoxycarbonyl-5-methoxycarbonyl-6-methyl-1,4-dihydropyrid-2-yl]methoxy}-2-hydroxy-2-methylpropane (0.25 g), N,N-dimethylformamide azine (0.21 g) and para-toluenesulphonic acid (10 mg) in toluene (10 ml) was heated under reflux for 1.5 hours and then partitioned between ethyl acetate and water. The layers were separated and the organic layer was washed with water, dried over Na2SO4 and evaporated. The residue was purified by chromatography on SiO2 (5 g) using dichloromethane plus 0-5% methanol as the eluant. Appropriate fractions were combined and evaporated and the residue triturated with ether. The resulting solid was collected, washed with ether and dried to give the title compound (0.18 g), m.p. 172°-176° C.

1. temperatureunder reflux for 1.5 hours
2. custompartitioned between ethyl acetate and water
3. customThe layers were separated
4. washthe organic layer was washed with water
5. dry with materialdried over Na2SO4
6. customevaporated
7. customThe residue was purified by chromatography on SiO2 (5 g)
8. customevaporated
9. customthe residue triturated with ether
10. customThe resulting solid was collected
11. washwashed with ether
12. customdried