HRID1098743

反应详情

EQUATION

反应方程式

HRID 1098743 的结构方程式

PROCEDURE

实验过程

To a solution of the compound from step 1 (630 mg, 1.79 mmol) in MeOH (30 mL) ammonium acetate (1.39 g, 17.9 mmol) was added. After stirring at ambient temperature overnight sodium cyanoborohydride (135.7 mg, 2.16 mmol) was added and the reaction was refluxed for 6 h. The solvent was evaporated and the solid, dissolved in ethyl acetate, was extracted with water. The organic layer was separated, washed with brine, dried over sodium sulphate, filtered and evaporated to give 606 mg (yield: 96%) of the crude product. LC/MS (method D) (M+H)+: 352

WORKUP

后处理

  1. additionwas added
  2. temperaturethe reaction was refluxed for 6 h
  3. customThe solvent was evaporated
  4. dissolutionthe solid, dissolved in ethyl acetate
  5. extractionwas extracted with water
  6. customThe organic layer was separated
  7. washwashed with brine
  8. dry with materialdried over sodium sulphate
  9. filtrationfiltered
  10. customevaporated