HRID439611

反应详情

EQUATION

反应方程式

HRID 439611 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of (R)-1-azabicyclo 2.2.1!heptan-3-one (U.S. Pat. No. 5,306,718) (2.22 g, 20 mmol) and hydroxylamine hydrochloride (1.39 g, 20 mmol) in MeOH (75 mL) is stirred at 25° C. for 18 hours. The solvent is removed under reduced pressure, the residual solid dissolves in saturated Na2CO3, and is extracted with CHCl3. The organic extracts are dried (Na2CO3), and concentrated to give the oxime. The aqueous layer is concentrated, and re-extracted with CHCl3 to yield additional product.

WORKUP

后处理

  1. additionA mixture of (R)-1-azabicyclo 2.2.1
  2. customThe solvent is removed under reduced pressure
  3. dissolutionthe residual solid dissolves in saturated Na2CO3
  4. extractionis extracted with CHCl3
  5. dry with materialThe organic extracts are dried (Na2CO3)
  6. concentrationconcentrated