反应详情

First, 3.0 g of 2,2-bis(6-benzyloxyhexyl)acetic acid, 2.8 g of 2,3-difluoro-4'-[11-hydroxyundecyl]oxybiphenyl, 2.2 g of triphenylphosphine, and 50 ml of tetrahydrofuran were placed in a 100 ml flask. Then, 1.4 g of diethyl azodicarboxylate was added dropwise to the mixture at 5° C. The resultant 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=1/9) to obtain 5 g of 11-[2,3-difluorobiphenyl-4'-yl]oxyundecyl 2,2-bis(6-benzyloxyhexyl)acetate (Y: 92.6%). The compound thus obtained had a purity of 98% by HPLC.

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