反应详情

温度

40 °C

To a stirred solution of 20.22 g (67 mmol) N-cyclopropyl-2-methyl-4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)benzamide in acetone (300 mL) were added 43.08 g (201 mmol) sodium periodate 134 mL ammonium acetate (134 mmol, 1M in water) and the mixture was stirred for 3 h at rt and 2 h at 40° C. 4 N HCl was added (32 mL) and the organic phase was removed in vaccuo. The mixture was extracted with ethyl acetate, and the organic phase was washed with water, dried and removed in vaccuo to yield 14.59 g (94.2%) of the title compound. 1H-NMR (400 MHz, DMSO-d6), δ [ppm]=0.44-0.52 (2H), 0.59-0.67 (2H), 2.26 (3H), 2.78 (1H), 7.18 (1H), 7.53-7.61 (2H), 8.01 (2H), 8.19 (1H).

1. customthe organic phase was removed in vaccuo
2. extractionThe mixture was extracted with ethyl acetate
3. washthe organic phase was washed with water
4. customdried
5. customremoved in vaccuo