反应详情

A solution of 2-(methylsulfonyl)thieno[2,3-d]pyrimidine (1.0 g, 4.67 mmol), 4-(2-aminoethyl)morpholine (1.8 g, 14.02 mmol), and 1-methyl-2-pyrrolidinone (1.5 mL) was heated to 100° C. overnight. The reaction mixture was cooled to RT and diluted with EtOAc (200 mL)/water (75 mL). The layers were separated, and the organic layer was washed successively with water (4×75 mL) and brine (1×75 mL). The organic layer was then dried over MgSO4, filtered and concentrated to give (1.2 g) of the crude product. The crude product was adsorbed onto a plug of silica gel and chromatographed through a Redi-Sep pre-packed silica gel column (40 g), eluting with a gradient of 5% to 95% MeOH in DCM to provide the title compound (1.02 g) MS (ES+): 265 (M+H)+.

1. customThe layers were separated
2. washthe organic layer was washed successively with water (4×75 mL) and brine (1×75 mL)
3. dry with materialThe organic layer was then dried over MgSO4
4. filtrationfiltered
5. concentrationconcentrated
6. customto give (1.2 g) of the crude product
7. customchromatographed through a Redi-Sep pre-packed silica gel column (40 g)
8. washeluting with a gradient of 5% to 95% MeOH in DCM