反应详情

温度

85 °C

To N-(5-chloro-2-fluorobenzyl)-2,2-dimethoxyacetamide (9.00 g, 34.3 mmol) were added conc. H2SO4 (25.0 mL, 465 mmol) and oleum (30%, 25.0 mL, 394 mmol). The mixture was heated at 85° C. for 2 h. Then, the reaction mixture was cooled to RT and poured slowly into a cold aqueous satd. solution of NaHCO3 (2.0 L) in a beaker with efficient stirring (Note: frothing occurs). The solid formed was filtered off, washed with water (50 mL), and dried in vacuo to give the title compound as yellow solid. 1H NMR (CDCl3, 300 MHz): δ=6.72 (t, J=8.4 Hz, 1H), 7.15 (s, 1H), 7.43 (dd, J=8.1, 4.2 Hz), 8.80 (s, 1H), —OH not visible. MS (ES+): m/z 197.72/199.77 [MH+]. HPLC: tR=2.58 min (ZQ2, polar—5 min).

1. temperatureThen, the reaction mixture was cooled to RT
2. additionpoured slowly into a cold aqueous satd
3. customThe solid formed
4. filtrationwas filtered off
5. washwashed with water (50 mL)
6. customdried in vacuo