反应详情

温度

65 °C

Water, 20 mL, was added to a mixture of 12.0 g (58.0 mmol) of 1-nitro-4-tert-butyl-2,6-dimethylbenzene dissolved in 160 mL of ethanol. To the stirring solution of 1-nitro-4-tert-butyl-2,6-dimethylbenzene was added CaCl2, 4.8 g (43.2 mmol), dissolved in 20 mL of water, followed by the addition of zinc powder, 50.0 g (76.5 mmol). The reaction was stirred overnight at 65° C., then cooled to ambient temperature and filtered. The filtrate was extracted three times with ether, and the organic layer was dried over MgSO4. Removal of the solvent gave 9.58 g (93%) of a brown oil. 1H NMR (300 MHz, CDCl3): δ=6.90, s, 2H, 3.40, broad singlet, 2H, 2.11, s, 6H, 1.21, s, 9H.

1. temperaturecooled to ambient temperature
2. filtrationfiltered
3. extractionThe filtrate was extracted three times with ether
4. dry with materialthe organic layer was dried over MgSO4
5. customRemoval of the solvent