反应详情

温度

20 °C

Sodium hydride (40 mg of 60% oil dispersion) was added at 0° C. to a solution of ethyl 4-(2,3-dihydro-6-methyl-4-oxo-5-phenyl-4H-1,3-oxazin-3-yl)-2-(4'-iodobutyl)-4-methyl-3-oxo-pentanoate (0.25 g) in N,N-dimethylformamide, and stirred at 20° C. for 2 hours. The mixture was diluted (ether),washed (brine), dried (MgSO4) and evaporated. The residue was purified by column chromatography (ethyl acetate/hexane 1:3) to give ethyl 1-[2-(2,3-dihydro-6-methyl-4-oxo-5-phenyl-4H-1,3-oxazin-3-yl)-2-methylpropionyl]cyclopentylcarboxylate (Compound 1, 0.14 g), NMR 1.21(3H, t), 1.4-1.6(8H, m), 1.7-1.8(2H, m), 1.91(3H, s), 2.1-2.2(2H, m), 2.4-2.5(2H, m), 3.60(2H, s), 4.14(2H, q), 5.16(2H, s), 7.2-7.4(5H, m).

1. dry with materialdried (MgSO4)
2. customevaporated
3. customThe residue was purified by column chromatography (ethyl acetate/hexane 1:3)