HRID565601

反应详情

EQUATION

反应方程式

HRID 565601 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 1-(3-methylphenyl)-1,3,8-triazaspiro[4.5]decan-4-one (0.25 g, 0.94 mmol), 1-(4-cyanobenzyl)-5-chloromethylimidazole hydrochloride salt (0.23 g, 0.94 mmol), and diisopropylethylamine (0.5 mL, 2.8 mmol) in absolute ethanol (5 mL) was heated under reflux overnight. The resulting mixture was concentrated under vacuum, and the residue was subjected to column chromatography on silica gel eluting with 5% methanol in ethyl acetate. The appropriate fractions were collected and concentrated. The residue was triturated with diethyl ether, and the white solid precipitated was collected by filtration to provide the title compound.

WORKUP

后处理

  1. temperatureunder reflux overnight
  2. concentrationThe resulting mixture was concentrated under vacuum
  3. customThe appropriate fractions were collected
  4. concentrationconcentrated
  5. customThe residue was triturated with diethyl ether
  6. customthe white solid precipitated
  7. filtrationwas collected by filtration