反应详情

温度

120 °C

To a mixture of (2S)-2-(aminomethyl)-4-(2,3-dihydro-1-benzofuran-7-yl)-1,1,1-trifluoro-4-methyl-2-pentanol (Intermediate 31, 87 mg, 0.3 mmol) and 4-bromo-6-methyl-1-phenyl-1H-indazole (Intermediate 33, 92 mg, 0.32 mmol) in toluene (3.5 mL) were added tris(dibenzylideneacetone)dipalladium(0) (35 mg, 0.04 mmol), racemic-BINAP (28 mg, 0.04 mmol) and sodium tert-butoxide (45 mg, 0.47 mmol). The mixture was heated in a microwave at 120° C. for 15 min and then cooled and partitioned between ethyl acetate (30 mL) and water (20 mL). The organic layer was separated, washed with water (20 mL), passed through a hydrophobic frit and evaporated. The residue was purified by two sequential SPE cartridge purifications eluting with a gradient of ethyl acetate:petroleum:ether (1:6 to 1:4) to give the title compound as a yellow foam (43 mg).

1. temperaturecooled
2. custompartitioned between ethyl acetate (30 mL) and water (20 mL)
3. customThe organic layer was separated
4. washwashed with water (20 mL)
5. customevaporated
6. customThe residue was purified by two sequential SPE cartridge purifications
7. washeluting with a gradient of ethyl acetate:petroleum:ether (1:6 to 1:4)