HRID2186727

反应详情

EQUATION

反应方程式

HRID 2186727 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

8-acetoxy-4-(2-(diphenylmethoxy)ethyl)-3-oxo-3,4-dihydro-2H-1,4-benzooxazine (630 mg) was dissolved in THF (10 ml), and a 1.0M borane THF solution (4.5 ml) was added to the resultant solution at 0° C., followed by stirring at room temperature for 4 hours. After water was added to the reaction solution to terminate reaction, the reaction solution was extracted with ethyl acetate. The resultant organic layer was washed with water, saturated sodium bicarbonate water, water and saturated brine, dried over sodium sulfate, and then concentrated. The residue was purified by medium-pressure column chromatography (solvent:ethyl acetate/cyclohexane=1/5) to obtain the colorless oily object compound (550 mg, yield 90%).

WORKUP

后处理

  1. customto terminate
  2. customreaction
  3. extractionthe reaction solution was extracted with ethyl acetate
  4. washThe resultant organic layer was washed with water, saturated sodium bicarbonate water, water and saturated brine
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated
  7. customThe residue was purified by medium-pressure column chromatography (solvent:ethyl acetate/cyclohexane=1/5)