HRID1511273

反应详情

EQUATION

反应方程式

HRID 1511273 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 91 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