反应详情

A solution of N-(2,5-dichlorobenzyl)-2,2-dimethoxyacetamide (1.0 g, 3.6 mmol) in sulfuric acid (18M; 4 mL) was stirred at 50° C. for 1 h. The reaction mixture was charged with ice and neutralized with NaHCO3. The aqueous mixture was extracted with 5% MeOH in DCM (3×), washed with NaHCO3, dried over sodium sulfate, filtered and concentrated to afford the title compound as yellow solid. MS (ES+): m/z=215.75/217.75 (3:1) [MH+]. HPLC: tR=2.76 min (ZQ2, polar—5 min).

1. extractionThe aqueous mixture was extracted with 5% MeOH in DCM (3×)
2. washwashed with NaHCO3
3. dry with materialdried over sodium sulfate
4. filtrationfiltered
5. concentrationconcentrated