反应详情

Into a 200 mL three-neck flask equipped with a stirrer, a thermometer, a cooling tube, and a calcium chloride tube, 20.0 g of ortho-phenylbenzyl alcohol, 100.0 g of anhydrous toluene, 13.2 g of triethylamine, and 7.8 mg of methoquinone were charged, and they were cooled to 10° C. or less using an ice bath. Into the flask, 11.8 g of acryloyl chloride was dropped over 30 minutes. The temperature was increased to room temperature and a reaction was caused to proceed for two hours. After the reaction, the reaction solution was poured into water and washed with a 5% NaOH aqueous solution and a saline solution, and the solvent, was distilled off to obtain an orange liquid. The orange liquid was purified with a silica gel column to obtain 20.44 g of ortho-phenylbenzyl acrylate. The obtained ortho-phenylbenzyl acrylate was a colorless, transparent liquid at ordinary temperature and had a refractive index of 1.5776 and a viscosity of 27 mPa·s at 25° C. The measurement result of 1H-NMR is shown below.

1. customInto a 200 mL three-neck flask equipped with a stirrer
2. temperaturethey were cooled to 10° C. or less
3. customAfter the reaction
4. washwashed with a 5% NaOH aqueous solution
5. distillationa saline solution, and the solvent, was distilled off
6. customto obtain an orange liquid
7. customThe orange liquid was purified with a silica gel column