反应详情

First, 4 g of 6-[2,3-difluorobiphenyl-4'-yl]oxyhexyl 2,2-bis(6-benzyloxyhexyl)acetate, 1.3 g of 10% Pd-C, and 150 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. The catalyst was filtered away and a filtrate was concentrated. Thereafter, the residue was purified by silica gel column chromatography (eluent: toluene/ethyl acetate=2/3) to obtain 2.6 g of 6-[2,3-difluorobiphenyl-4'-yl]oxyhexyl 2,2-bis(6-hydroxyhexyl)acetate (Y: 90%). The compound thus obtained had a purity of 99.3% by HPLC.

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