反应详情

A 250 ml round bottom flask was charged with a mixture of 6-amino-1-hydroxy-2,1-benzoxaborolane hydrochloride (1 g, 5.4 mmol, 1 eq), triethylamine (2.3 ml, 16.2 mmol, 3 eq) and dichloromethane (100 ml). 2-Chloro-4-fluorobenzoyl chloride (1.14 g, 5.9 mmol, 1.1 eq) was added, and the reaction mixture was allowed to stir at room temperature overnight. Aqueous hydrochloric acid (1 M, 50 ml) was added to the mixture and the suspension was vigorously mixed. The resulting white precipitate was then collected by vacuum filtration and dried under vacuum. LCMS (m/e) 306 (M+H). 1H NMR (400 MHz, DMSO-d6) δ ppm 4.96 (s, 2H) 7.29-7.45 (m, 2H) 7.59 (dd, J=9.0, 2.3 Hz, 1H) 7.63-7.78 (m, 2H) 8.15 (d, J=1.8 Hz, 1H) 9.25 (s, 1H) 10.53 (s, 1H). Amount Obtained: 1.1 g, 67% yield.

1. additionthe suspension was vigorously mixed
2. filtrationThe resulting white precipitate was then collected by vacuum filtration
3. customdried under vacuum
4. customAmount Obtained