反应详情

First, 2.8 g of 13-[trans-4-(2,3-difluorophenyl)cyclohexyl]tridecyl 2,2-bis(6-hydroxyhexyl)acetate, 1 g of triethylamine, and 30 ml of benzene were placed in a 100 ml flask. A small amount of benzene in which 0.9 g of acryloyl chloride was dissolved was added dropwise to the reaction mixture under ice water cooling. The reaction mixture was allowed to warm to room temperature and stirred for 3 hours. The reaction mixture was poured into water, and an organic layer was extracted with ether. The ether layer was washed with diluted hydrochloric acid and water in this order, and then dried over anhydrous sodium sulfate. The solvent was distilled away. The residue was purified by silica gel column chromatography (eluent: ethyl acetate/toluene=1/20) to obtain 1.12 g of 13-[trans-4-(2,3-difluorophenyl)cyclohexyl]tridecyl 2,2-bis(6-acryloyloxyhexyl)acetate (Y: 33%). The compound thus obtained was liquid at room temperature. The compound had a purity of 99.6% by HPLC and of 1 spot by TLC.

1. additionwas added dropwise to the reaction mixture under ice water cooling
2. extractionan organic layer was extracted with ether
3. washThe ether layer was washed with diluted hydrochloric acid and water in this order
4. dry with materialdried over anhydrous sodium sulfate
5. distillationThe solvent was distilled away
6. customThe residue was purified by silica gel column chromatography (eluent: ethyl acetate/toluene=1/20)