反应详情

A solution of 8-cyclopropylmethyl-2-(4-fluorophenyl)-3-(2-methanesulfonylpyrimidin-4-yl)imidazo[1,2-a]pyrazine (3.00 g, 7.08 mmol) and 3-amino-2,2-dimethylpropan-1-ol (TCI-US, 3.65 g, 35.4 mmol) in ACN (100 mL) was heated at about 85° C. for about 2 d. After cooling to ambient temperature, a precipitate formed, which was filtered off, washed with ACN, dried in vacuo and purified by silica gel chromatography with heptane/EtOAc (gradient 50-100% EtOAc, then isocratic 100% EtOAc). After concentration, the residue was three times re-dissolved in DCM and re-concentrated, resulting in a colorless foam, which was dried in a vacuum oven for about 16 h at about 55° C. and about 21 Torr to give 1.809 g (56%) of the title compound as a colorless solid: LC/MS (Table 1, Method g) Rt=3.01 min; MS m/z: 447.2 (M+H)+.

1. customa precipitate formed
2. filtrationwhich was filtered off
3. washwashed with ACN
4. customdried in vacuo
5. custompurified by silica gel chromatography with heptane/EtOAc (gradient 50-100% EtOAc
6. concentrationAfter concentration
7. dissolutionre-dissolved in DCM
8. concentrationre-concentrated
9. customresulting in a colorless foam, which
10. customwas dried in a vacuum oven for about 16 h at about 55° C.