HRID1055030

反应详情

EQUATION

反应方程式

HRID 1055030 的结构方程式

PROCEDURE

实验过程

7-chloro-2-(2-(1-(4-methoxybenzyl)-5-(pyrrolidin-1-yl)-1H-1,2,4-triazol-3-yl)ethyl)quinoxaline (17 mg, 37.9 μmol, Eq: 1.00) was stirred in trifluoroacetic acid (173 mg, 117 μl, 1.51 mmol, Eq: 40) with anisole (81.9 mg, 82.7 μl, 757 μmol, Eq: 20) at 120° C. overnight. The mixture was made basic by addition of sodium hydroxide 2N aq. and extracted three times with 1,2-dichloromethane, dried over magnesium sulfate, filtered and evaporated. The crude material was applied on silica gel and purified by column chromatography to give 7-Chloro-2-[2-(5-pyrrolidin-1-yl-1H-[1,2,4]triazol-3-yl)-ethyl]-quinoxaline (2.2 mg, 17.7%) as off-white solid. MS: m/z=329.12 (M+H+)

WORKUP

后处理

  1. extractionextracted three times with 1,2-dichloromethane
  2. dry with materialdried over magnesium sulfate
  3. filtrationfiltered
  4. customevaporated
  5. custompurified by column chromatography