HRID1022581

反应详情

EQUATION

反应方程式

HRID 1022581 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 2-chloro-N-[(3RS)-3-(3,4-dichlorophenyl)-3-hydroxy-4-methoxybutyl]acetamide (2.10 g) in THF (150 ml) was added sodium tert-butoxide (592 mg), and the mixture was heated under reflux for 10 min. The reaction mixture was quenched with water, and the mixture was extracted with ethyl acetate. The organic layer was washed with brine, and dried over anhydrous magnesium sulfate, and the solvent was evaporated. The residue was purified by silica gel column chromatography (eluent; hexane:ethyl acetate (1:1)-ethyl acetate:methanol (4:1)) to give the title compound (2.13 g).

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 10 min
  3. customThe reaction mixture was quenched with water
  4. extractionthe mixture was extracted with ethyl acetate
  5. washThe organic layer was washed with brine
  6. dry with materialdried over anhydrous magnesium sulfate
  7. customthe solvent was evaporated
  8. customThe residue was purified by silica gel column chromatography (eluent; hexane:ethyl acetate (1:1)-ethyl acetate:methanol (4:1))