HRID40188

反应详情

EQUATION

反应方程式

HRID 40188 的结构方程式

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

A mixture of N4-((6-phenyl-[1,2,4]triazolo[4,3-b]pyridazin-3-yl)methyl)pyridine-3,4-diamine (0.0650 g, 0.20 mmol), triethyl orthoformate (5.0 ml, 30 mmol), and p-TsOH (0.0039 g, 0.020 mmol) was heated at 60° C. After 2 h reaction is complete. Reaction was concentrated. Took up in DMSO and purified on RPHPLC. Fractions containing product were treated with 9% sodium carbonate and volatiles removed. Collected product by filtration. MS m/z=328.1 [M+1]+. Calc'd for C18H13N7: 327.3.

WORKUP

后处理

  1. customAfter 2 h reaction
  2. customReaction
  3. concentrationwas concentrated
  4. custompurified on RPHPLC
  5. additionFractions containing product
  6. additionwere treated with 9% sodium carbonate and volatiles
  7. customremoved
  8. filtrationCollected product by filtration