反应详情

温度

90 °C

Sulfuric acid (18 M; 2.0 mL, 36 mmol.) was added to N-(5-chloro-2,4-difluorobenzyl)-2,2-dimethoxyacetamide (708 mg, 2.53 mmol) at rt. The solution was stirred at 90° C. overnight. After that time, the mixture was poured into ice and basified with NaOH (10 N) until pH=6-7 forming a solid. The solid was filtered off, washed with water, and dried in vacuo to give the title compound as a yellow solid. 1H NMR (400 MHz, CDCl3): δ=6.94 (t, J=9.2 Hz, 1H), 7.48 (s, 1H), 9.04 (s, 1H). MS(ES+): m/z=215.47/217.76 (45/100) [MH+]. HPLC: tR=2.67 min (polar—5 min, ZQ3).

1. additionAfter that time, the mixture was poured into ice
2. customforming a solid
3. filtrationThe solid was filtered off
4. washwashed with water
5. customdried in vacuo