反应详情

A solution of 0.75 g (2.8 mmoles) 6-nitro-5-ethyl-2-ethoxy-3,1-benzoxazin-4-one in 35 mL ethyl acetate was transferred to a Parr bottle. 0.40 g (0.38 mmoles) of 10% Pd/C catalyst was added. The sample was hydrogenated on a Parr shaker at ambient temperature and 1 atm pressure for 3 hours. The catalyst was removed by filtration through a pad of Celite. The filtrate was concentrated in vacuo to produce a bright yellow solid. There was obtained 0.58 g (86% yield) of 6-amino-5-ethyl-2-ethoxy-3,1-benzoxazin-4-one. NMR(CDCl3): 1.22 (t,3H,J=7.5 Hz), 1.42(t,3H,J=7.2 Hz), 3.14(q,2H,J=7.5 Hz), 4.44(q,2H,J=7.2 Hz), 7.09(d,1H,J=8.7 Hz), 7.14(d,1H,J=8.7 Hz). MS(m/z): 234(M+).

1. customwas hydrogenated on a Parr shaker at ambient temperature
2. customThe catalyst was removed by filtration through a pad of Celite
3. concentrationThe filtrate was concentrated in vacuo
4. customto produce a bright yellow solid