HRID40225

反应详情

EQUATION

反应方程式

HRID 40225 的结构方程式

PROCEDURE

实验过程

A 16 mm test tube was charged with (6-phenyl-[1,2,4]triazolo[4,3-b][1,2,4]triazin-3-yl)methanol (0.500 g, 2.20 mmol), Reactant 2 (0.951 ml, 4.40 mmol), DBU (0.663 ml, 4.40 mmol), and toluene (8.16 ml, 77.0 mmol), flushed with argon, sealed, then stirred at room temperature for 3 hours. The dark maroon mixture was concentrated and the resulting dark purple/black oil was purified by column chromatography using a gradient of 3-5% MeOH/DCM over 20 minutes. 3-(azidomethyl)-6-phenyl-[1,2,4]triazolo[4,3-b][1,2,4]triazine was isolated as a brown solid.

WORKUP

后处理

  1. customflushed with argon
  2. customsealed
  3. concentrationThe dark maroon mixture was concentrated
  4. customthe resulting dark purple/black oil was purified by column chromatography
  5. customover 20 minutes