HRID584751

反应详情

EQUATION

反应方程式

HRID 584751 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

Potassium carbonate (279 mg, 2.02 mmol) and potassium iodide (335 mg, 2.02 mmol) was added to a solution of 1,5-bis(4-methoxyphenyl)-1H-1,2,4-triazol-3-ol (200 mg, 0.673 mmol) in dimethylformamide (2 mL). After 5 minutes stirring, 3-(chloromethyl)-1,2,4-oxadiazole (239 mg, 2.02 mmol) was added to the mixture and the mixture was heated at 100° C. for 1 hour. After cooling, ethyl acetate and water were poured into the mixture. The organic layer was separated, washed with water and brine, and dried over magnesium sulfate. The solvent was removed under reduced pressure. The residue was purified by preparative-TLC (toluene-ethyl acetate 4:1). The desired product was triturated with isopropylether, isolated by filtration, and dried in vacuo to give 3-({[1,5-bis(4-methoxyphenyl)-1H-1,2,4-triazol-3-yl]oxy}methyl)-1,2,4-oxadiazole (110 mg, 43.1% yield).

WORKUP

后处理

  1. temperatureAfter cooling
  2. customThe organic layer was separated
  3. washwashed with water and brine
  4. dry with materialdried over magnesium sulfate
  5. customThe solvent was removed under reduced pressure
  6. customThe residue was purified by preparative-TLC (toluene-ethyl acetate 4:1)
  7. customThe desired product was triturated with isopropylether
  8. customisolated by filtration
  9. customdried in vacuo