HRID1695810
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 stirred solution of 4-methyl-4H-benzo[1,4]oxazin-3-one (2.18 g, 13.37 mmol) in THF (5 mL) was added borane-tetrahydrofuran complex (4.02 g, 46.8 mmol) at room temperature. After stirring the solution for 2 h, the reaction mixture was refluxed for 4 h. After complete conversion, reaction mixture was quenched by adding MeOH (10 mL) and evaporated the solvents. The residue obtained was extracted with ethyl acetate (30×2 mL) and the organic layer was washed with water (20 mL), brine (20 mL) and evaporation of solvent gave 4-methyl-3,4-dihydro-2H-benzo[1,4]oxazine 2.0 g.
WORKUP
后处理
- temperaturethe reaction mixture was refluxed for 4 h
- customAfter complete conversion, reaction mixture
- customwas quenched
- additionby adding MeOH (10 mL)
- customevaporated the solvents
- customThe residue obtained
- extractionwas extracted with ethyl acetate (30×2 mL)
- washthe organic layer was washed with water (20 mL), brine (20 mL) and evaporation of solvent