反应详情

温度

50 °C

To a mixture of N-{[6-(4,4-dimethylcyclohexyl)-2-methylthieno[2,3-d]pyrimidin-4-yl]methyl}tetrahydro-2H-thiopyran-4-amine-1,1-dioxide hydrochloride (100 mg), CH3I (16 μL) and DMF (2.0 mL) was added K2CO3 (60 mg), followed by stirring at 50° C. overnight. The reaction mixture was left to be cooled, and a saturated aqueous NH4Cl solution was added thereto, followed by extraction with EtOAc. The organic layer was washed sequentially with water and brine, and dried over MgSO4. The residue was purified by silica gel column. The obtained purified product was dissolved in EtOAc, and 4 M HCl/EtOAc (55 μL) was added dropwise thereto. The precipitate was collected by filtration and then dried to obtain N-{[6-(4,4-dimethylcyclohexyl)-2-methylthieno[2,3-d]pyrimidin-4-yl]methyl}-N-methyltetrahydro-2H-thiopyran-4-amine 1,1-dioxidehydrochloride (69 mg).

1. waitThe reaction mixture was left
2. temperatureto be cooled
3. extractionfollowed by extraction with EtOAc
4. washThe organic layer was washed sequentially with water and brine
5. dry with materialdried over MgSO4
6. customThe residue was purified by silica gel column
7. customThe obtained purified product
8. dissolutionwas dissolved in EtOAc
9. addition4 M HCl/EtOAc (55 μL) was added dropwise
10. filtrationThe precipitate was collected by filtration
11. customdried