反应详情

First, 10.9 g of 2,3-difluoro-1-[trans-4-{13-benzyloxy-1-tridecenyl}cyclohexyl]benzene, 1 g of 10% Pd-C, 50 ml of ethanol, and 50 ml of ethyl acetate were placed in a 500 ml autoclave. The mixture was stirred at room temperature for 5 days under a hydrogen pressure of 8 kg/cm2. A catalyst was filtered away and a filtrate was concentrated. Thereafter, the residue was purified by silica gel column chromatography (eluent: toluene/ethyl acetate=4/1) and recrystallized from acetone to obtain 5.7 g of 2,3-difluoro-1-[trans-4-(13-hydroxytridecyl)cyclohexyl]benzene (Y: 64%). The compound thus obtained had a purity of 97.2% by GC and 99.8% by HPLC.

1. filtrationA catalyst was filtered away
2. concentrationa filtrate was concentrated
3. customThereafter, the residue was purified by silica gel column chromatography (eluent: toluene/ethyl acetate=4/1)
4. customrecrystallized from acetone