Potassium Phosphate, Tribasic → 5-(1-hydroxy-3-methylbutyl)-1-methyl-3-(3-((tetrahydro-2H-pyran-2-yl)oxy) propyl)-6-(3-(trifluoromethoxy)phenyl)thieno[2,3-d]pyrimidine-2,4(1H,3H)-dione

関与物質

反応条件

反応手順

To a solution of 6-bromo-5-(1-hydroxy-3-methylbutyl)-1-methyl-3-(3-((tetrahydro-2H-pyran-2-yl)oxy)propyl)thieno[2,3-d]pyrimidine-2,4(1H,3H)-dione (70 mg, 0.143 mmol) in dioxane (2 mL) was added (3-(trifluoromethoxy)phenyl)boronic acid (58.9 mg, 0.286 mmol), Pd(PPh3)4 (10 mg) and aq. 2M K3PO4 (0.4 mL). The reaction was heated at 85° C. for 2 h then cooled to RT and filtered. The filtrate was diluted with DCM (10 mL) and water (10 mL). The organic layer was dried over Na2SO4 and concentrated to a residue which was purified by chromatography eluted with PE/EA (10:1 to 5:1) to give 5-(1-hydroxy-3-methylbutyl)-1-methyl-3-(3-((tetrahydro-2H-pyran-2-yl)oxy)propyl)-6-(3-(trifluoromethoxy)phenyl)thieno[2,3-d]pyrimidine-2,4(1H,3H)-dione (50 mg, 61.2% yield) as a solid. LCMS: [MH+-THP] 487 and TR=2.079 min.

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