HRID1907758
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
- 130 °C
PROCEDURE
实验过程
To a solution of 1-[(4-Pyridyl)methyl]piperazine (1.00 g, 5.6 mmol) in DMSO (4.5 mL) in a pressure vessel was added t-butyl-4-fluorobenzoate (1.05 g, 5.4 mmol) followed by potassium carbonate (0.74 g, 5.4 mmol). The pressure vessel was closed and the mixture was stirred at 130° C. for 21 h. The mixture was diluted with EtOAc (300 mL) and water (50 mL). The organic layer was separated, washed with a saturated NaHCO3 solution, brine, dried over MgSO4, and concentrated in vacuo. The residue obtained was purified by flash chromatography using 0-5% MeOH in DCM to afford the title compound 338 as a pink solid (1.34 g, 71% yield).
WORKUP
后处理
- customThe pressure vessel was closed
- customThe organic layer was separated
- washwashed with a saturated NaHCO3 solution, brine
- dry with materialdried over MgSO4
- concentrationconcentrated in vacuo
- customThe residue obtained
- customwas purified by flash chromatography