Water → Florpyrauxifen-benzyl

関与物質

反応手順

Benzyl 4-amino-6-(4-chloro-2-fluoro-3-methoxyphenyl)-5-fluoropicolinate (2.07 g, 5.12 mmol) was slurried in acetonitrile (20 mL) in a scintillation vial. 1,3-Dichloro-5,5-dimethylhydantoin (554 mg, 2.181 mmol) was added as a solid, and the reaction mixture was stirred at reflux for 1 h. After cooling to room temperature, water (40 mL) was added to precipitate the product. The solid was collected on a Buchner funnel and washed with water. Drying under vacuum at 55° C. gave a white solid (2.187 g, 97%): 1H NMR (400 MHz, CDCl3) δ 7.50-7.41 (m, 2H, aromatic), 7.41-7.20 (m, 5H, aromatic), 5.42 (s, 2H, CH2Ph), 4.92 (br s, 2H, NH2), 3.97 (d, J=1.2 Hz, 3H, OMe); 19F{1H} NMR (CDCl3) δ −128.19 (d, J=33.9 Hz, F2′), −137.79 (d, J=33.8 Hz, F5).

情報源と証拠