HRID1003800

反应详情

EQUATION

反应方程式

HRID 1003800 的结构方程式

PROCEDURE

实验过程

1-Benzyl-4-hydroxypyrazole (2 g, 11.5 mmol), potassium carbonate(3.2 g, 23 mmol), and (2s)-glycidyl-3-nitrobenzenesulfonate (2.98 g, 11.5 mmol) were slurried in actone (300 ml) at reflux for 17 hours. The acetone was removed in vacuo, the residue extracted from brine with chloroform, and dried over sodium sulfate. The solvent was removed again and the residue purified by column chromatography (silica gel, chloroform→1% methanol/chloroform) to yield product (1.8 g, 68%). MS, NMR.

WORKUP

后处理

  1. temperatureat reflux for 17 hours
  2. customThe acetone was removed in vacuo
  3. extractionthe residue extracted from brine with chloroform
  4. dry with materialdried over sodium sulfate
  5. customThe solvent was removed again
  6. customthe residue purified by column chromatography (silica gel, chloroform→1% methanol/chloroform)