HRID383820
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
- 70 °C
PROCEDURE
实验过程
To a solution of piperazine-1-carboxylic acid tent-butyl ester (0.750 g, 4.03 mmol) in dry acetonitrile (20 mL) grounded potassium carbonate (0.486 mL, 8.05 mmol) was added followed by the product mixture from Example 38a (1.134 g) and the reaction was heated at 70° C. under argon over night. The acetonitrile was evaporated and DCM and water was added. The layers were separated and the aq phase was extracted with DCM (3×). The combined organic phases were dried (Na2SO4), filtered and evaporated. The crude mixture was purified by flash chromatography (heptane/EtOAc 75/25 to 0/100) to give 0.823 g (55%) of the title compound.
WORKUP
后处理
- additionwas added
- customThe acetonitrile was evaporated
- additionDCM and water was added
- customThe layers were separated
- extractionthe aq phase was extracted with DCM (3×)
- dry with materialThe combined organic phases were dried (Na2SO4)
- filtrationfiltered
- customevaporated
- customThe crude mixture was purified by flash chromatography (heptane/EtOAc 75/25 to 0/100)