反应详情

温度

25 °C

A solution of (D3) (2.30 g, 6.40 mmol), ammonium formate (2.02 g, 32.10 mmol) and 10% palladium on carbon (1 g) in methanol (100 mL) was heated at 70° C. for 3 h, then cooled to 25° C. and filtered through Celite. Evaporation in vacuo gave an oil which was suspended in dichloromethane and washed with saturated sodium carbonate solution. The organic layer was removed, dried (Na2SO4), and the solvents evaporated in vacuo to give the title compound as a yellow oil (1.2 g). 1H NMR (CDCl3) δ: 2.05-2.20 (2H, m), 2.68 (3H, s), 2.85-2.95 (2H, m), 3.00-3.15 (2H, m), 4.35-4.45 (1H, m), 5.85-5.90 (1H, m), 7.40-7.50 (2H, m), 7.62 (1H, s), 7.72 (1H, d, J=8.2 Hz), 7.91 (1H, d, J=7.6 Hz), 9.14 (1H, s).

1. filtrationfiltered through Celite
2. customEvaporation in vacuo
3. customgave an oil which
4. washwashed with saturated sodium carbonate solution
5. customThe organic layer was removed
6. dry with materialdried (Na2SO4)
7. customthe solvents evaporated in vacuo