HRID1622562
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
- 125 °C
PROCEDURE
实验过程
A mixture of (S)-tert-butyl(3-bromopyridin-2-yl)(4-(trifluoromethyl)-phenyl)methylcarbamate (Intermediate 40, Step 5) (0.711 g, 1.649 mmol), 2-(tributylstannyl)pyridine (0.910 g, 2.473 mmol), and (Ph3P)4Pd (0.381 g, 0.330 mmol) in 1,4-dioxane (10 mL) was heated by microwave at 125° C. for 30 min. The reaction mixture was then cooled, concentrated, and purified by ISCO (silica gel, 0-60% EtOAc/hexanes). The residue was dissolved in DCM (3 mL) and hydrogen chloride (3.30 mL, 13.19 mmol, 4.0 M in 1,4-dioxane) was added. After stirring for 2 h, the mixture was concentrated to dryness to give the title compound. MS (ESI pos. ion) m/z: 330.0 (M+H).
WORKUP
后处理
- temperatureThe reaction mixture was then cooled
- concentrationconcentrated
- custompurified by ISCO (silica gel, 0-60% EtOAc/hexanes)
- dissolutionThe residue was dissolved in DCM (3 mL)
- concentrationthe mixture was concentrated to dryness