1160294-85-8

white powder

Step 1: Synthesis of 3-bromo-6,9-diphenyl-9H-carbazole In a 300 mL Erlenmeyer flask, 4.8 g (15 mmol) of 3,9-diphenyl-9H-carbazole and 250 mL of mixed solvent (ethyl acetate: toluene = 4:1) were added. The mixture was stirred for 30 min to ensure complete dissolution. Subsequently, 2.7 g (15 mmol) of N-bromosuccinimide (NBS) was slowly added and the reaction mixture was continuously stirred for 48 hours. After completion of the reaction, the reaction mixture was washed sequentially with saturated sodium bicarbonate solution and saturated brine. The organic layer was separated and dried with anhydrous magnesium sulfate. After drying, the magnesium sulfate was removed by filtration and the filtrate was concentrated to obtain an oil. A small amount of ethanol was added to the oil and the solid was induced to precipitate by ultrasonic treatment. The precipitated solid was collected by diafiltration to give 5.4 g of white powdery product in 90% yield.

[1] Patent: WO2009/72587, 2009, A1. Location in patent: Page/Page column 243-244
[2] Patent: TW2017/2233, 2017, A. Location in patent: Paragraph 0197; 0200; 0201
[3] Patent: WO2012/121561, 2012, A1. Location in patent: Page/Page column 26-27