反应详情

First, 3 g of 2,3-difluoro-1-[trans-4-(13-hydroxytridecyl)cyclohexyl]benzene, 3 g of 2,2-bis(6-benzyloxyhexyl)acetic acid, 2.2 g of triphenylphosphine, and 30 ml of tetrahydrofuran were placed in a 100 ml flask. Then, 1.5 g of ethyl azodicarboxylate was added dropwise to the reaction mixture under ice water cooling. The reaction mixture was allowed to warm to room temperature and stirred for 2 hours. The reaction mixture was concentrated, and the residue was purified by silica gel column chromatography (eluent: hexane/ethyl acetate=9/1) to obtain 5.4 g of 13-[trans-4-(2,3-difluorophenyl)cyclohexyl]tridecyl 2,2-bis(6-benzyloxyhexyl)acetate (Y: 97%). The compound thus obtained had a purity of 93.7% by HPLC.

1. concentrationThe reaction mixture was concentrated
2. customthe residue was purified by silica gel column chromatography (eluent: hexane/ethyl acetate=9/1)