反应详情

温度

40 °C

1-amino-2-methylanthraquinone (300 g) is slurried with 1500 ml of HOAc in a 5-liter flask. The temperature is raised to 40° C. Neat bromine (405 g) is added over a 21/2 hours with stirring at 40°-50° C. The mixture is stirred for 20 additional minutes and filtered. The solids so recovered are washed with HOAc and water and sucked dry with an aspirator and transferred to a reaction flask along with 150 g of NaHSO3 and 1.5 liters of water. The mixture is gradually heated to 90° C. (over two hours) with stirring to give 1-amino-2-methyl-4-bromoanthraquinone (AMBAX) as a solid which is recovered from the reaction mixture by filtration in 90% yield, rinsed with water and dried overnight at 155° C. and 1 mm Hg absolute vacuum. ##STR23##

1. stirringThe mixture is stirred for 20 additional minutes
2. filtrationfiltered
3. customThe solids so recovered
4. washare washed with HOAc and water
5. customsucked dry with an aspirator
6. customtransferred to a reaction flask along with 150 g of NaHSO3 and 1.5 liters of water
7. temperatureThe mixture is gradually heated to 90° C. (over two hours)
8. stirringwith stirring