HRID1924006

反应详情

EQUATION

反应方程式

HRID 1924006 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Platinum(IV) oxide (2.75 g, 12.1 mmole) was added to a suspension, saturated with nitrogen, of CaO (9.30 g, 166 mmole) and [1,2,4]-triazolo[1,5-a]pyrazine (18.1 g, 151 mmole) in methoxyethanol (150 ml). The reaction mixture was stirred for 21.5 hours under a hydrogen atmosphere. The catalyst was filtered off through filter earth and washed with DCM/ethanol (9:1). The filtrate was concentrated, and the solvent was removed firstly with toluene and then with 2-propanol. The residue was taken up in ethyl acetate, filtered again through filter earth, washed with ethyl acetate, and concentrated. The residue was washed with hot 2-propanol and concentrated in vacuo.

WORKUP

后处理

  1. filtrationThe catalyst was filtered off
  2. filtrationthrough filter earth
  3. washwashed with DCM/ethanol (9:1)
  4. concentrationThe filtrate was concentrated
  5. customthe solvent was removed firstly with toluene
  6. filtrationfiltered again
  7. filtrationthrough filter earth
  8. washwashed with ethyl acetate
  9. concentrationconcentrated
  10. washThe residue was washed with hot 2-propanol
  11. concentrationconcentrated in vacuo