反应详情

First, 5.8 g of 16-[2,3-difluorobiphenyl-4'-yl]oxyhexadecyl 2,2-bis(6-benzyloxyhexyl)acetate, 1.8 g of 10% Pd-C, and 100 ml of tetrahydrofuran were placed in a 300 ml autoclave. The mixture was stirred at room temperature for 2 days under a hydrogen pressure of 10 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=7/3) to obtain 3.9 g of 16-[2,3-difluorobiphenyl-4'-yl]oxyhexadecyl 2,2-bis(6-hydroxyhexyl)acetate (Y: 85.5%). The compound thus obtained had a purity of 99.2% by HPLC and an m.p. of 45.2° C. to 48.8° C.

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=7/3)