HRID732146

反应详情

EQUATION

反应方程式

HRID 732146 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

[5-(3-cyanophenyl)-1,2,4-oxadiazol-3-yl]methyl methanesulfonate (0.278 g; 0.99 mmol) and 3-pyridin-4-yl-5,6,7,8-tetrahydro[1,2,4]triazolo[4,3-a]pyrimidine (0.220 g; 1.09 mmol) were dissolved in butanone (20 ml) and potassium carbonate (0.275 g; 1.99 mmol) was added portionwise. The mixture was heated at reflux for 18 h before cooling to r.t. This mixture was concentrated in vacuo and DCM (20 ml) was added. The mixture was washed with water, dried (Na2SO4), evaporated and purified using prep. HPLC chromatography to give the title compound (5.4 mg). 1H NMR: 8.77 (m, 2H), 8.41 (s, 1H), 8.34 (d, 1H), 7.87 (d, 1H), 7.68 (t, 1H), 7.56 (m, 2H) 5.51 (s, 2H), 4.09 (m, 2H), 3.62 (m, 2H), 2.19 (m, 2H).

WORKUP

后处理

  1. temperatureThe mixture was heated
  2. temperatureat reflux for 18 h
  3. concentrationThis mixture was concentrated in vacuo and DCM (20 ml)
  4. additionwas added
  5. washThe mixture was washed with water
  6. dry with materialdried (Na2SO4)
  7. customevaporated
  8. custompurified