HRID633499

反应详情

EQUATION

反应方程式

HRID 633499 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

0.11 cm3 of acetic anhydride is added to a mixture of 202 mg of 3-chloro[1,2,4]triazolo[4,3-b]pyridazin-6-amine in 5 cm3 of pyridine at 0° C. The temperature is allowed to rise to 20° C. over 6 h, then 0.05 cm3 of acetic anhydride is again added and stirring is maintained for 24 h. The precipitate formed is spin-filter-dried and then washed with ethyl ether and pentane. This solid is purified by chromatography on Biotage Quad 12/25 (KP-SIL, 60 A; 32-63 μM), elution being carried out with a gradient of dichloromethane/methanol of 100/0 to 90/10. 41 mg of N-(3-chloro[1,2,4]triazolo[4,3-b]pyridazin-6-yl)acetamide are thus obtained in the form of a white powder, the characteristics of which are as follows:

WORKUP

后处理

  1. temperatureis maintained for 24 h
  2. customThe precipitate formed
  3. customis spin-filter-dried
  4. washwashed with ethyl ether and pentane
  5. customThis solid is purified by chromatography on Biotage Quad 12/25 (KP-SIL, 60 A
  6. wash32-63 μM), elution