反应详情

温度

35 °C

A solution of (239 g, 1.2 mol) 4-tert-butyl-1-methyl-2-nitro-benzene (M. S. Carpenter, W. M. Easter, T. F. Wood, J. Org. Chem. (1951), 586) in MeOH (1.0 L) was treated with Raney nickel (25 g) in a Parr shaker. The apparatus was sealed under hydrogen pressure to 52 psi, heated to 35° C. for 15 hours, and cooled to room temperature. The apparatus was vented and the contents filtered. The filtrate was concentrated in vacuo and distilled, collecting the major fraction (75°-85° C., 1.0 torr). 1H NMR (CDCl3) δ 1.26 (s, 9 H), 2.11 (s, 3 H), 3.54 (bs, 2 H), 6.69 (d, 1 H), 6.72 (dd, 1 H), 6.96 (d, 1 H).

1. customThe apparatus was sealed under hydrogen pressure to 52 psi
2. temperaturecooled to room temperature
3. filtrationthe contents filtered
4. concentrationThe filtrate was concentrated in vacuo
5. distillationdistilled
6. customcollecting the major fraction (75°-85° C., 1.0 torr)