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 bottom flask was charged with 2-(6-tert-butyl-8-fluoro-1-oxo-phthalazin-2(1H)-yl)-4-chloronicotinaldehyde 103b (150 mg, 0.43 mmol), (S)-3-(5-(2-ethyl-4-(oxetan-3-yl)piperazin-1-yl)pyridin-2-ylamino)-1-methyl-5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)pyridin-2(1H)-one (206 mg, 0.43 mmol), PdCl2(dppf) (33 mg, 0.04 mmol), K3PO4 (202 mg, 0.86 mmol), NaOAc (71 mg, 0.86 mmol), and CH3CN (10 mL), H2O (2 mL). After three cycles of vacuum/argon flush, the mixture was heated at 100° C. for 3 h. It was then filtered and the filtrate was evaporated in vacuo. The residue was purified by flash column chromatography eluting with 1:3 petroleum/ethyl acetate to afford 112a as a yellow solid (146 mg, 49%). LCMS: [M+H]+ 693
WORKUP
后处理
- customAfter three cycles of vacuum/argon flush
- filtrationIt was then filtered
- customthe filtrate was evaporated in vacuo
- customThe residue was purified by flash column chromatography
- washeluting with 1:3 petroleum/ethyl acetate