反应详情

温度

25 °C

LiOH.H2O (8.8 mmol, 4.0 equiv.) was added at 0° C. to a solution of 7-tert-butyl 2-ethyl-5,6-dihydroimidazo[1,2-a]pyrazine-2,7(8H)-dicarboxylate (2.2 mmol, 1.0 equiv.) in methanol/water (2.5:1, 35 ml), and the mixture was then stirred for 2 h at 25° C. When the reaction was complete (TLC monitoring), the methanol was removed in vacuo, the residue was diluted with water (40 ml), and extraction with ethyl acetate (2×40 ml) was carried out. The aqueous phase was then adjusted to pH 2-3 with 1N HCl solution, and the resulting solid was filtered out. The solid was taken up in toluene, and the solvent was then removed in vacuo (2×) to yield the desired product in the form of a white solid. Yield: 68%.

1. customthe methanol was removed in vacuo
2. additionthe residue was diluted with water (40 ml), and extraction with ethyl acetate (2×40 ml)
3. filtrationthe resulting solid was filtered out
4. customthe solvent was then removed in vacuo (2×)