反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 80 °C
PROCEDURE
实验过程
A mixture of Trifluoro-methanesulfonic acid 3-((R)-1-tert-butoxycarbonylamino-ethyl)-phenyl ester (0.340 g, 0.921 mmol), 1-methylpiperazine (0.37 g, 3.68 mmol), Pd2(dba)3 (0.042 g, 0.046 mmol), 2-(di-tert-butylphosphino)-biphenyl (0.054 g, 0.184 mmol), and potassium phosphate (0.273 g, 1.29 mmol) in 20 mL of 1,4 dioxane was heated at 80° C. in a sealed tube for 12 hours. After completion of the reaction, the reaction mixture was cooled to room temperature and diluted with ethyl acetate (100 mL) and the washed with water (20 mL). The aqueous layer was extracted with ethyl acetate (2×50 mL), and the combined organic layers were dried over magnesium sulfate and concentrated in vacuo to afford the crude title compound.
WORKUP
后处理
- customAfter completion of the reaction
- temperaturethe reaction mixture was cooled to room temperature
- washthe washed with water (20 mL)
- extractionThe aqueous layer was extracted with ethyl acetate (2×50 mL)
- dry with materialthe combined organic layers were dried over magnesium sulfate
- concentrationconcentrated in vacuo