HRID40187

反应详情

EQUATION

反应方程式

HRID 40187 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of N4-((6-phenyl-[1,2,4]triazolo[4,3-b]pyridazin-3-yl)methyl)pyridine-3,4-diamine (0.0640 g, 0.202 mmol) in HOAc (5 mL) was added sodium nitrite (0.0153 g, 0.222 mmol) in water (2 mL). Stirred for 1 h. Concentrated. Took up in DMSO and purified on RPHPLC. Took fractions containing product and made basic with 9% sodium carbonate and removed volatiles in vacuo. Product crashed out and was isolated by filtration. MS m/z=329.2[M+1]+. Calc'd for C17H12N8: 328.3.

WORKUP

后处理

  1. concentrationConcentrated
  2. custompurified on RPHPLC
  3. additionTook fractions containing product
  4. customremoved volatiles in vacuo
  5. customwas isolated by filtration