反应详情

A mixture of 5-(2-(methylthio)pyrimidin-4-yl)thiophene-2-sulfonyl chloride (200 mg, 0.65 mmol), morpholine (62 mg, 0.72 mmol) and triethylamine (78 mg, 0.78 mmol) in tetrahydrofuran (5 mL) was stirred at rt for 2 days. Water (50 mL) was added and the mixture was extracted with ethyl acetate (3×50 mL). The combined organic layer was washed with brine (50 mL), dried over anhydrous sodium sulfate and filtered. The solvent was evaporated in vacuo and the residue was washed with diethyl ether (2 mL) to give a white solid. The solid was dissolved in 30 mL of acetone-water (1:1) and then oxone (2 g) was added. After stirring at rt for 20 h the mixture was concentrated in vacuo to remove the acetone. The white precipitate was filtered off, washed with water and dried to afford the title compound (186 mg, 73%). MS (M+H)+ 390.

1. extractionthe mixture was extracted with ethyl acetate (3×50 mL)
2. washThe combined organic layer was washed with brine (50 mL)
3. dry with materialdried over anhydrous sodium sulfate
4. filtrationfiltered
5. customThe solvent was evaporated in vacuo
6. washthe residue was washed with diethyl ether (2 mL)
7. customto give a white solid
8. stirringAfter stirring at rt for 20 h the mixture
9. concentrationwas concentrated in vacuo
10. customto remove the acetone
11. filtrationThe white precipitate was filtered off
12. washwashed with water
13. customdried