反应详情

Stannous chloride dihydrate (4.39 g, 19.4 mmol) was added to a solution of diethyl 2-(4-nitrobenzyl)-2-methylmalonate (3.00 g, 9.70 mmol) in EtOH (30 ml) and stirred at reflux for 3 h. Water and ethyl acetate were added and the solution was basified with triethyl amine adjusted an pH˜9. The salts were filtered and washed with ethyl acetate. The organic layer was separated from the filtrate and washed with water, brine solution, dried over anhydrous sodium sulfate, filtered and concentrated under reduced pressure to afford 2.20 g (81.4%) of diethyl 2-(4-aminobenzyl)-2-methylmalonate as brown oil.

1. temperatureat reflux for 3 h
2. filtrationThe salts were filtered
3. washwashed with ethyl acetate
4. customThe organic layer was separated from the filtrate
5. washwashed with water, brine solution
6. dry with materialdried over anhydrous sodium sulfate
7. filtrationfiltered
8. concentrationconcentrated under reduced pressure