HRID1264312
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
PROCEDURE
实验过程
To a solution of ethyl 4-(2-oxo-2H-pyridin-5-yl)benzoate (1.24 g, 5.10 mmoles, reference example 36f) in allyl alcohol (50 mL) was added titanium (IV) isopropoxide. The resulting mixture was heated to 70° C. for seven hours at which point more titanium (IV) isopropoxide (3 mL) was added. After 18 hours the heat was removed and 1N HCl solution (50 mL) was added followed by extraction with CH2Cl2 (200 mL). The organic layer was isolated and concentrated to give the title compound in quantitative yield. MS (ion spray) m/z 256 (M+H)+.
WORKUP
后处理
- additionwas added
- customAfter 18 hours the heat was removed
- addition1N HCl solution (50 mL) was added
- extractionfollowed by extraction with CH2Cl2 (200 mL)
- customThe organic layer was isolated
- concentrationconcentrated