反应详情

Formic acid (67) (0.921 g, 20 mmol) and triethylamine (2.226 g, 22 mmol) were combined and stirred for 30 minutes. Compound (61) (0.299 g, 1 mmol) was then added and stirred for three days. The solution was dissolved in 10 mL of ethyl acetate and the precipitate was filtered and washed with 10 mL diethylether. The combined filtrate was then washed with brine and dried with sodium sulfate. The solvent was evaporated to get dark brown viscous oil. 1H NMR (400 MHz, CDCl3): δ 1.44 (s, 12H), 1.80 (s, 4H), 4.57 (s, 4H), 8.11 (s, 2H).

1. stirringstirred for three days
2. filtrationthe precipitate was filtered
3. washwashed with 10 mL diethylether
4. washThe combined filtrate was then washed with brine
5. dry with materialdried with sodium sulfate
6. customThe solvent was evaporated
7. customto get dark brown viscous oil