反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 100 °C
PROCEDURE
实验过程
A 50-mL round-bottomed flask equipped with a reflux condenser was charged with 2-(6-tert-butyl-8-fluoro-1-oxophthalazin-2(1H)-yl)-4-chloronicotinaldehyde 103b (216 mg, 1 eq., 0.60 mmol), 131d (446 mg, 2 eq., 1.2 mmol), Pd2(dba)3 (55 mg, 0.1 eq., 0.060 mmol), Cy3P (67 mg, 0.4 eq., 0.24 mmol), Cs2CO3 (395 mg, 2 eq., 1.2 mmol), water (0.5 mL), and dioxane (10 mL). After three cycles of vacuum/N2 flush, the reaction mixture was stirred at 100° C. for 2 hrs. It was then cooled to room temperature and filtered. The filtrate was evaporated under reduced pressure and the resulting residue was purified by silica-gel column chromatography eluting with 4:1 petroleum ether/ethyl acetate to afford 131e (272 mg, 80%) as a brown solid. MS-ESI: [M+H]+ 569.8
WORKUP
后处理
- customA 50-mL round-bottomed flask equipped with a reflux condenser
- customAfter three cycles of vacuum/N2 flush
- temperatureIt was then cooled to room temperature
- filtrationfiltered
- customThe filtrate was evaporated under reduced pressure
- customthe resulting residue was purified by silica-gel column chromatography
- washeluting with 4:1 petroleum ether/ethyl acetate