反应详情

温度

60 °C

72 mg (0.64 mmol) of potassium tert-butoxide were suspended in 1 ml of dry dimethoxyethane. 270 mg (1.29 mmol) of [2-(4-chlorophenyl)-1,3-oxazol-4-yl]methanol and 50 mg (0.13 mmol) of the compound from Example 48A were then added in succession. The reaction mixture was stirred at 60° C. for 2 h and then cooled to RT and stirred at this temperature for 8 h. 5 ml of water and 1 ml of 2N acetic acid were added to the reaction mixture. A precipitate is formed, which was filtered off with suction. The residue was purified by preparative HPLC (column: YMC GEL ODS-AQ S-5/15 μm; mobile phase gradient: acetonitrile/water 10:90→95:5). Removal of the solvent on a rotary evaporator gave the product as a solid.

1. temperaturecooled to RT
2. stirringstirred at this temperature for 8 h
3. customA precipitate is formed
4. filtrationwhich was filtered off with suction
5. customThe residue was purified by preparative HPLC (column: YMC GEL ODS-AQ S-5/15 μm; mobile phase gradient: acetonitrile/water 10:90→95:5)
6. customRemoval of the solvent
7. customon a rotary evaporator