HRID571046
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
PROCEDURE
实验过程
A suspension of 4-butylaniline (0.6 g, 4.1 mmol) and 5-(benzyloxy)-4-oxo-4H-pyran-2-carboxylic acid (1.0 g, 4.1 mmol) in a 1:1 mixture of AcOH:water (4 mL) was heated in a sealed reaction vessel at 120° C. for 72 h. After cooling to room temperature, the reaction mixture was concentrated under reduced pressure, diluted with 10 mL 10% aq. NaOH, and extracted with EtOAc (3×10 mL). The organic fractions were pooled, dried (Na2SO4), and concentrated under reduced pressure to provide 3-(benzyloxy)-1-(4-butylphenyl)pyridin-4(1H)-one, which was used in the subsequent step without further purification. LC/MS (M+H)+ 334.
WORKUP
后处理
- concentrationthe reaction mixture was concentrated under reduced pressure
- additiondiluted with 10 mL 10% aq. NaOH
- extractionextracted with EtOAc (3×10 mL)
- dry with materialdried (Na2SO4)
- concentrationconcentrated under reduced pressure