HRID1109718
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
To a solution of 7-fluoro-6-isocyanato-4-propargyl-2H-1,4-benzoxazin-3(4H)-one (2.5 g) and methyl 2-hydroxy-3-methyl-3-butenoate (1.3 g) in benzene (50 ml), triethylamine (0.5 g) was added at room temperature. The resulting mixture was refluxed for 1 hour, cooled to room temperature, combined with water and extracted with ethyl acetate. The organic layer was washed with water, dried over magnesium sulfate and concentrated. The residue was purified by silica gel column chromatography using a mixture of toluene and ethyl acetate as the eluent to give Compound No. 72 (2.9 g). nD25.0 1.4868
WORKUP
后处理
- temperatureThe resulting mixture was refluxed for 1 hour
- extractionextracted with ethyl acetate
- washThe organic layer was washed with water
- dry with materialdried over magnesium sulfate
- concentrationconcentrated
- customThe residue was purified by silica gel column chromatography
- additiona mixture of toluene and ethyl acetate as the eluent
- customto give Compound No