HRID593002
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 (S)-tert-butyl 4-(6-aminopyridin-3-yl)-3-methylpiperazine-1-carboxylate 191f (580 mg, 2.0 mmol), 253a (1.36 g, 4.0 mmol), Pd2(dba)3 (180 mg, 0.20 mmol), Xantphos (230 mg, 0.40 mmol), Cs2CO3 (1.3 g, 4.0 mmol), and dioxane (20 mL). After three cycles of vacuum/argon flush, the mixture was heated at 100° C. for 2 h. 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 253b (1.0 g, 91%) as yellow solid. MS-ESI: [M+H]+ 551.2
WORKUP
后处理
- customA 50-mL round-bottomed flask equipped with a reflux condenser
- customAfter three cycles of vacuum/argon 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