反应详情

316 g of 2-bromo-5-nitro-p-xylene were dissolved in 3000 ml of methanol, freshly produced Raney nickel (about 4 g) was added under a vigorous stream of N2, and the mixture was heated to reflux with vigorous stirring. 275 ml of hydrazine hydrate (80% in water) were then slowly added dropwise. When the dropwise addition was complete (duration about 5 hours), the mixture was refluxed for about a further 6 hours. The catalyst was filtered off, the methanol was removed in a rotary evaporator, the residue was taken up in ethyl acetate, and the solution was washed by shaking with water, dried and re-evaporated in a rotary evaporator. The resultant crude product was recrystallized from heptane, giving 238 g (87%) of pale-green crystals.

1. temperaturethe mixture was heated
2. temperatureto reflux with vigorous stirring
3. additionWhen the dropwise addition
4. temperaturethe mixture was refluxed for about a further 6 hours
5. filtrationThe catalyst was filtered off
6. customthe methanol was removed in a rotary evaporator
7. washthe solution was washed
8. customdried
9. customre-evaporated in a rotary evaporator
10. customThe resultant crude product was recrystallized from heptane