反应详情

245.0 g of 3A was mixed with 1.6 liters of glacial acetic acid, and the resulting solution was stirred at 8°-10° C. while 109.6 g of 90% aqueous nitric acid was added (two hours). The mixture was stirred at 10°-15° C. for five hours, poured over ice water and extracted with ether/hexane. The extract was washed with water, dried and stripped to dryness. The residue was stirred with 3 liters of hexane and the hexane solution was filtered through silica gel. The filtrate was held at -20° C. for 16 hours, filtered, and the filtrate was concentrated to one liter, charcoaled, then held at -30° to -35° C. for two hours and filtered. The solid products were combined to give 3-chloro-4-methyl-6-nitrophenol (3B).

1. additionwas added (two hours)
2. extractionextracted with ether/hexane
3. washThe extract was washed with water
4. customdried
5. stirringThe residue was stirred with 3 liters of hexane
6. filtrationthe hexane solution was filtered through silica gel
7. waitThe filtrate was held at -20° C. for 16 hours
8. filtrationfiltered
9. concentrationthe filtrate was concentrated to one liter
10. waitheld at -30° to -35° C. for two hours
11. filtrationfiltered