反应详情

First, 2.47 g of 2,2-bis(6-benzyloxyhexyl)acetic acid, 1.85 g of 2,3-difluoro-4'-[6-hydroxyhexyl]oxybiphenyl, 1.6 g of triphenylphosphine, and 50 ml of tetrahyrofuran were placed in a 100 ml flask. Then, 1.1 g of diethyl azodicarboxylate was added dropwise to the reaction mixture at 5° C. Thereafter, the reaction mixture was allowed to warm to room temperature and stirred for 8 hours. The reaction mixture was concentrated, and the residue was purified by silica gel column chromatography (eluent: ethyl acetate/hexane=1/4) to obtain 4 g of 6-[2,3-difluorobiphenyl-4'-yl]oxyhexyl 2,2-bis(6-benzyloxyhexyl)acetate (Y: 97.8%). The compound thus obtained had a purity of 99% by HPLC.

1. concentrationThe reaction mixture was concentrated
2. customthe residue was purified by silica gel column chromatography (eluent: ethyl acetate/hexane=1/4)