1,2-Aceanthrylenedione, 6-bromo- synthesis

Yield:53336-66-6 75%

Reaction Conditions:

with Aluminum Chloride in carbon disulfide; for 4 h;Cooling with ice;Inert atmosphere;

Steps:

1.1

1) Dissolve 9-bromoanthraquinone (1.03g, 4mmol) and oxalyl chloride solution (1.92ml, 10mmol) in carbon disulfide (8~10ml) with stirring at 0°C in an ice bath under nitrogen, and then add three Aluminum chloride (0.81g, 6mmol) was reacted for 2 hours; carbon disulfide (8 ~ 10ml) and aluminum trichloride (0.64g, 4.8mmol) were added, and the ice bath was kept at 0C and the reaction was stirred again for 2 hours, then the ice bath was removed. The reaction is stirred under warm conditions (8-10) hours; 60 ml of 1-2 M hydrochloric acid solution is added and the temperature is raised to 50° C. and maintained for 10 minutes; after cooling to room temperature, filtration is carried out while washing with water and then 5-10% w. After washing with /w sodium hydroxide solution and finally washing with water, the crude extract (filter residue) was placed in a vacuum oven and dried at 50°C for 48 hours; the resulting light brown solid was purified by silica gel column chromatography to give a brown solid of 6-bromoacetic acid. Ether-1,2-dione (0.93 g, yield 75%).

References:

CN107488147,2017,A Location in patent:Paragraph 0067