HRID1863941

反应详情

EQUATION

反应方程式

HRID 1863941 的结构方程式

PROCEDURE

实验过程

A suspension of 40 mg (0.196 mmol) of 3-(trifluoromethyl)[1,2,4]triazolo[4,3-a]pyrazine 7-oxide in 0.9 mL of phosphorus oxychloride was stirred at reflux for 2.5 h. The cooled solution was concentrated to dryness. Purification of the residue by preparative HPLC (C18 reverse phase column, 10-70% acetonitrile in water containing 0.05% trifluoroacetic acid) and then by flash chromatography on silica gel (10-30% ethyl acetate in hexanes) yielded the title compound as a white solid. LC-MS 223 (M+1).

WORKUP

后处理

  1. temperatureat reflux for 2.5 h
  2. concentrationThe cooled solution was concentrated to dryness
  3. customPurification of the residue by preparative HPLC (C18 reverse phase column, 10-70% acetonitrile in water containing 0.05% trifluoroacetic acid) and then by flash chromatography on silica gel (10-30% ethyl acetate in hexanes)