反应详情

First, 3.4 g of 16-[2,3-difluorobiphenyl-4'-yl]oxyhexadecyl 2,2-bis(6-hydroxyhexyl)acetate, 3 g of triphenylphosphine, 0.9 g of acrylic acid, and 30 ml of tetrahydrofuran were placed in a 100 ml flask. Then, 10 ml of a solution in which 2 g of ethyl azodicarboxylate was dissolved in tetrahydrofuran was added dropwise to the mixture under ice water cooling. The resultant mixture was allowed to warm to room temperature and stirred for 3 hours. The reaction mixture was concentrated. Thereafter, the residue was purified by silica gel column chromatography (eluent: ethyl acetate/toluene=1/20) and recrystallized from hexane to obtain 2.7 g of 16-[2,3-difluorobiphenyl-4'-yl]oxyhexadecyl 2,2-bis(6-acryloyloxyhexyl)acetate (Y: 59.7%). The compound thus obtained had a purity of 99% by HPLC and of 1 spot by TLC. The compound had an m.p. of 33.8° C. to 35.5° C.

1. additionwas added dropwise to the mixture under ice water cooling
2. concentrationThe reaction mixture was concentrated
3. customThereafter, the residue was purified by silica gel column chromatography (eluent: ethyl acetate/toluene=1/20)
4. customrecrystallized from hexane