HRID1415546
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A solution of 3.7 g. (15.4 mmoles) of 9-acetoxyxanthene and 2.2 g. (15.5 mmoles) of 1-ethyl-3-methylaminopiperidine in 80 ml. of benzene was refluxed under nitrogen for 22.5 hours. It was then cooled to room temperature, washed with aqueous sodium bicarbonate solution, and dried over potassium carbonate. After removal of solvent in vacuo, the residue was dissolved in 25 ml. of petroleum ether and filtered from a small amount of crystals. The filtrate was then concentrated in vacuo and chromatographed on silica gel (ether solvent) to give N-methyl-N-(N-ethyl-3-piperidinyl)-9-xanthenylamine.
WORKUP
后处理
- washwashed with aqueous sodium bicarbonate solution
- dry with materialdried over potassium carbonate
- customAfter removal of solvent in vacuo
- dissolutionthe residue was dissolved in 25 ml
- filtrationof petroleum ether and filtered from a small amount of crystals
- concentrationThe filtrate was then concentrated in vacuo
- customchromatographed on silica gel (ether solvent)