反应 #90030
ord-b9d0a98fe4834385af7afb06cd46afe8
反应方程式
反应物
溶剂
反应条件
后处理
- 1其他The mixture was subjected to reduced pressure under ultrasonication treatment
- 2其他by flushing with nitrogen gas
- 3其他degassed
- 4温度the mixture was cooled to room temperature
- 5workup.ADDITIONadded with water (250 ml)
- 6workup.STIRRINGfurther stirred for 30 min
- 7过滤The precipitates were filtered
- 8洗涤washed with water (50 ml)
- 9洗涤They were further washed with CH3CN (50 ml)
实验过程
To trifluoro-methanesulfonic acid 3-cyano-6,6-dimethyl-11-oxo-6,11-dihydro-5H-benzo[b]carbazol-8-yl ester (Compound B1, 7.80 g, 18.0 mmol), 4-(4,4,5,5-tetramethyl-[1,3,2]dioxaborolan-2-yl)-3,6-dihydro-2H-pyridine-1-carboxylic acid tert-butyl ester (6.11 g, 19.8 mmol, 1.1 eq.), Pd(PPh3)2Cl2 (630 mg, 0.898 mmol, 0.05 eq.), and sodium carbonate (5.71 g, 53.9 mmol, 3.0 eq.), DME (125 ml) and water (25 ml) were added. The mixture was subjected to reduced pressure under ultrasonication treatment, followed by flushing with nitrogen gas. This procedure was repeated five times and then degassed. After further stirring at 80° C. for 2 hr under nitrogen atmosphere, the mixture was cooled to room temperature, added with water (250 ml), and further stirred for 30 min. The precipitates were filtered and washed with water (50 ml). They were further washed with CH3CN (50 ml) to obtain the target compound as a crude product (gray powder, 7.54 g, 90%).