HRID1003800
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
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
- temperatureat reflux for 17 hours
- customThe acetone was removed in vacuo
- extractionthe residue extracted from brine with chloroform
- dry with materialdried over sodium sulfate
- customThe solvent was removed again
- customthe residue purified by column chromatography (silica gel, chloroform→1% methanol/chloroform)