HRID1068180

反应详情

EQUATION

反应方程式

HRID 1068180 的结构方程式

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

  1. temperaturewas refluxed for 1 hour
  2. customThe solvent was removed under reduced pressure
  3. customthe residue purified by silica gel chromatography (300 mL column)
  4. washElution with 0-5% MeOH in dichloromethane