Toluene → (R)-2-(4-(9-Hydroxy-2-(3-hydroxy-3-methylbutoxy)-9-(trifluoromethyl)-9H-fluoren-4-yl)-1H-pyrazol-1-yl)-2-methylpropanamide

Participants

Reaction Conditions

Reaction Steps

To 2-{4-[(9R)-9-hydroxy-2-(3-hydroxy-3-methylbutyloxy)-9-(trifluoromethyl)-9H-fluoren-4-yl]-1H-pyrazol-1-yl}-2-methylpropanamide monohydrate (compound (2h)) (22.63 g) obtained in the previous step was added toluene (340 ml). The reaction mixture was stirred at an oil bath temperature of 130° C. for 2 hr under a nitrogen atmosphere with removing water by a Dean-Stark apparatus. The reaction mixture was further stirred at an oil bath temperature of 70° C. for 1.5 hr, allowed to cool to room temperature, and stirred overnight. The precipitated solid was collected by filtration, and washed with toluene (100 ml). The obtained solid was dried under reduced pressure at room temperature for 3 days, and further dried under reduced pressure at 60° C. for 1 day to give the title compound (21.5 g).

Provenance & Evidence