Potassium Phosphate, Tribasic → 8-({[Tert-butyl(dimethyl)silyl]oxy}methyl)-8-methyl-3-{1-[4'-(pyrrolidin-1-ylcarbonyl)biphenyl-4-yl]cyclopropyl}-5,6,8,9-tetrahydro[1,2,4]triazolo[4,3-d][1,4]thiazepine

関与物質

反応手順

A solution of the compound (324 mg, 0.7 mmol) obtained in Example 1-2), 4-(pyrrolidin-1-ylcarbonyl)phenylboronic acid (32 mg, 0.77 mmol), tris(dibenzylideneacetone)dipalladium(0) (32 mg, 0.04 mmol), tricyclohexylphosphine (23 mg, 0.08 mmol), and tripotassium phosphate (260 mg, 1.19 mmol) in dioxane (2 mL) and water (1 mL) was stirred at 140° C. for 2 h under microwave irradiation. The reaction mixture was purified by silica gel chromatography (Isco Combiflash, 12 g, methanol:ethyl acetate=0:100 to 20:80, gradient) to obtain the title compound (385 mg, 91%) as a yellow oily substance.

情報源と証拠