HRID584749

反应详情

EQUATION

反应方程式

HRID 584749 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
45 °C

PROCEDURE

实验过程

Dimethylcarbamic chloride was added to a mixture of 1,5-bis(4-methoxyphenyl)-1H-1,2,4-triazol-3-ol (200 mg, 0.673 mmol) and pyridine (0.114 ml, 1.41 mmol) in dichloromethane (5 ml). Then the solution was stirred at 45° C. for 17 hours. Water and ethyl acetate were poured into the mixture and 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 column chromatography (hexane-ethyl acetate 1:2). The desired product was washed with isopropyl ether to give 1,5-bis(4-methoxyphenyl)-1H-1,2,4-triazol-3-yl dimethylcarbamate. (88 mg, 35.5% yield)

WORKUP

后处理

  1. customthe organic layer was separated
  2. washwashed with water and brine
  3. dry with materialdried over magnesium sulfate
  4. customThe solvent was removed under reduced pressure
  5. customThe residue was purified by column chromatography (hexane-ethyl acetate 1:2)
  6. washThe desired product was washed with isopropyl ether