반응 #90030
ord-b9d0a98fe4834385af7afb06cd46afe8
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후처리
- 1기타The mixture was subjected to reduced pressure under ultrasonication treatment
- 2기타by flushing with nitrogen gas
- 3기타degassed
- 4온도the mixture was cooled to room temperature
- 5workup.ADDITIONadded with water (250 ml)
- 6workup.STIRRINGfurther stirred for 30 min
- 7여과The precipitates were filtered
- 8세척washed with water (50 ml)
- 9세척They were further washed with CH3CN (50 ml)
실험 절차
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%).