HRID1068180
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
A mixture of 1.52 g 1-benzyl-4-hydrazinopiperidine and 2.0 g of ethyl 2-benzylacetoacetate in 20 mL of xylenes was refluxed for 1 hour. The solvent was removed under reduced pressure and the residue purified by silica gel chromatography (300 mL column). Elution with 0-5% MeOH in dichloromethane gave 1.61 g of product, 1-benzyl-4-(4-benzyl-5-methyl-1H-pyrazol-3(2H)-on-2-yl)-piperidine. ESI-MS 362.2 (M+H); HPLC A: 2.05 min.
WORKUP
后处理
- temperaturewas refluxed for 1 hour
- customThe solvent was removed under reduced pressure
- customthe residue purified by silica gel chromatography (300 mL column)
- washElution with 0-5% MeOH in dichloromethane