反应详情

温度

130 °C

A mixture of 2-[5′-fluoro-5-(3,5-bis-trifluoromethyl-phenylamino)-3′-trifluoromethyl-biphenyl-3-yl]-4-methyl-pentanoic acid methyl ester (57 mg, 0.096 mmol), potassium tert-butoxide (58 mg, 0.52 mmol), methyl iodide (60 μL, 0.11 mmol), dioxane (2 mL) and N-methylpyrrolidinone (0.2 mL) was stirred with microwave irradiation for 15 min at 130° C. The mixture was concentrated in vacuo, suspended in 1M HCl (20 mL) and extracted with diethyl ether (2×20 mL). The combined organic layer was washed with brine, dried (MgSO4), concentrated in vacuo and purified by flash column chromatography (silica, 0-5% diethyl ether in petroleum ether) to afford the title product as a colourless solid (33 mg, 56%). RT=5.24 min.

1. concentrationThe mixture was concentrated in vacuo
2. extractionextracted with diethyl ether (2×20 mL)
3. washThe combined organic layer was washed with brine
4. dry with materialdried (MgSO4)
5. concentrationconcentrated in vacuo
6. custompurified by flash column chromatography (silica, 0-5% diethyl ether in petroleum ether)