HRID338098

反应详情

EQUATION

反应方程式

HRID 338098 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Powdered zinc (43.7 g, 669 mmol) is added to a solution of benzyl 6a-phenyl-3,3a,4,6-tetrahydro-1H-pyrrolo[3,4-c]isoxazole-5-carboxylate (31 g, 96 mmol) in acetic acid (310 mL) and the mixture is stirred for 30 minutes. Ethyl acetate (500 mL) is added and the mixture is filtered through diatomaceous earth. The solvent is removed under vacuum and the crude product is re-dissolved in ethyl acetate. Water is added to the solution and the pH is adjusted to 10 with 2 M NaOH. The solution is filtered through diatomaceous earth, the layers are separated, and the organic layer is dried over magnesium sulfate, and concentrated to give the title compound (31 g, 99%). ES/MS (m/e): 327 (M+H).

WORKUP

后处理

  1. filtrationthe mixture is filtered through diatomaceous earth
  2. customThe solvent is removed under vacuum
  3. dissolutionthe crude product is re-dissolved in ethyl acetate
  4. additionWater is added to the solution
  5. filtrationThe solution is filtered through diatomaceous earth
  6. customthe layers are separated
  7. dry with materialthe organic layer is dried over magnesium sulfate
  8. concentrationconcentrated