反应详情

To 2'-acetylamino-4',5'-methylenedioxy-2-chloroacetophenone (0.9 g, 3.53 mmol) or an equivalent amount of 2'-pivoylamino-4',5'-methylenedioxy-2-chloroacetophenone in ethanol (60 mL) at about 5° C. is added, dropwise, conc. HCI (12.5 mL, 149.7 mmol). The reaction mixture is then heated at reflux for about an hour, then poured over 2 N NaOH/ice (80 mL/60 g) and washed with ethyl acetate (3 ×70 mL). The organic portions are combined and washed with brine (50 mL), dried (anhydrous sodium sulfate) and concentrated in vacuo to yield a greenish-yellow solid. This solid is recrystallized from ethyl acetate/isopropanol/hexane, treated with activated charcoal, to yield 2'-amino-4',5'-methylenedioxy-2-chloroacetophenone (0.39 g, 52% of theory).

1. temperatureThe reaction mixture is then heated
2. temperatureat reflux for about an hour
3. washwashed with ethyl acetate (3 ×70 mL)
4. washwashed with brine (50 mL)
5. dry with materialdried (anhydrous sodium sulfate)
6. concentrationconcentrated in vacuo
7. customto yield a greenish-yellow solid
8. customThis solid is recrystallized from ethyl acetate/isopropanol/hexane
9. additiontreated with activated charcoal