HRID389985

反应详情

EQUATION

反应方程式

HRID 389985 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a solution of 4-benzylpiperazine-2,6-dione (which may be prepared in accordance with the experimental described in Example 4, step 1; 2.0 g, 9.8 mmol) in a mixture of methanol/H2O (65 mL/28 mL) were added a solution of HCl 1N in methanol (23.8 mL) and Pd/C (10% wet, 0.2% wt., 400 mg). The reaction mixture was degassed 3 times with hydrogen/vacuum prior to its overnight stirring under hydrogen (P=1 atm). The reaction mixture was then filtered on Clarcel® and washed with methanol. The filtrate was finally concentrated to dryness and the residue was precipitated from a mixture of methanol and ether. The title product was obtained as a beige solid (418 mg, 28%).

WORKUP

后处理

  1. customThe reaction mixture was degassed 3 times with hydrogen/vacuum
  2. filtrationThe reaction mixture was then filtered on Clarcel®
  3. washwashed with methanol
  4. concentrationThe filtrate was finally concentrated to dryness
  5. customthe residue was precipitated from a mixture of methanol and ether