反应详情

To a solution of 8-cyclopropylmethyl-2-(4-fluorophenyl)-3-(2-methylsulfanylpyrimidin-4-yl)imidazo[1,2-a]pyrazine (5.16 g, 13.2 mmol) in DCM (50 mL) and MeOH (50 mL) was added a solution of Oxone® (16.2 g, 26.4 mmol) in water (50 mL). After about 4 h of rapid stirring, the mixture was neutralized with saturated Na2CO3 solution and extracted with DCM. The combined organic phase was dried over Na2SO4 and concentrated. The crude material was purified by silica gel chromatography with heptane/EtOAc (gradient 50-100% EtOAc). After concentration, the residue was three times re-dissolved in DCM and re-concentrated to give 4.77 g (85%) of the title compound as a yellowish solid: LC/MS (Table 1, Method g) Rt=2.68 min; MS m/z: 424.1 (M+H)+.

1. extractionextracted with DCM
2. dry with materialThe combined organic phase was dried over Na2SO4
3. concentrationconcentrated
4. customThe crude material was purified by silica gel chromatography with heptane/EtOAc (gradient 50-100% EtOAc)
5. concentrationAfter concentration
6. dissolutionre-dissolved in DCM
7. concentrationre-concentrated