HRID64491

反应详情

EQUATION

反应方程式

HRID 64491 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To 301 mg of 8-[(2,6-difluorobenzyl)oxy]-N-[2,2-dimethyl-5-(3-methylphenyl)-1,3-dioxan-5-yl]-2-methylimidazo[1,2-a]pyridine-3-carboxamide were added 3 ml of dioxane, 3 ml of methanol, and 6 ml of 1 M hydrochloric acid, followed by stirring for 14 hours. To the reaction mixture were added a saturated aqueous sodium hydrogen carbonate solution, water, and ethyl acetate under ice-cooling to carry out a layer separation operation. The organic layer was washed with a saturated aqueous sodium hydrogen carbonate solution and saturated brine in this order, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure and the obtained residue was purified by silica gel column chromatography. To the obtained purified product were added hexane and ethyl acetate, and the insoluble material was collected by filtration and dried to obtain 172 mg of 8-[(2,6-difluorobenzyl)oxy]-N-[1,3-dihydroxy-2-(3-methylphenyl)propan-2-yl]-2-methylimidazo[1,2-a]pyridine-3-carboxamide.

WORKUP

后处理

  1. temperaturecooling
  2. customa layer separation operation
  3. washThe organic layer was washed with a saturated aqueous sodium hydrogen carbonate solution and saturated brine in this order
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customThe solvent was evaporated under reduced pressure
  6. customthe obtained residue was purified by silica gel column chromatography
  7. customTo the obtained purified product
  8. additionwere added hexane and ethyl acetate
  9. filtrationthe insoluble material was collected by filtration
  10. customdried