HRID458692

反应详情

EQUATION

反应方程式

HRID 458692 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
10 °C

PROCEDURE

实验过程

Acetone cyanohydrin (17 grams, 200 mmol) was added to 400 mL of a 2M solution of NH3 in methanol and the resulting mixture stirred under N2 for 4 days. The solvent was removed in vacuo and the remaining residue dissolved in 250 mL of H2O. After cooling to 10° C., the solution was treated with Na2CO3 (21 grams, 200 mmol) and 95% benzyloxy chloroformate (33 mL, 230 mmol) and stirring continued overnight. Ethyl acetate was added and the mixture transferred to a seperatory funnel. The aqueous layer was removed and the ethyl acetate solution washed with saturated NaHCO3. After drying over Na2SO4 the solvent was removed to yield a solid which was triturated with hexanes to provide the title compound.

WORKUP

后处理

  1. customThe solvent was removed in vacuo
  2. dissolutionthe remaining residue dissolved in 250 mL of H2O
  3. stirringstirring continued overnight
  4. customthe mixture transferred to a seperatory funnel
  5. customThe aqueous layer was removed
  6. washthe ethyl acetate solution washed with saturated NaHCO3
  7. dry with materialAfter drying over Na2SO4 the solvent
  8. customwas removed
  9. customto yield a solid which
  10. customwas triturated with hexanes