HRID1258802

反应详情

EQUATION

反应方程式

HRID 1258802 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperaturethe reaction mixture was refluxed for 4 h
  2. customAfter complete conversion, reaction mixture
  3. customwas quenched
  4. additionby adding MeOH (10 mL)
  5. customevaporated the solvents
  6. customThe residue obtained
  7. extractionwas extracted with ethyl acetate (30×2 mL)
  8. washthe organic layer was washed with water (20 mL), brine (20 mL) and evaporation of solvent