HRID1415546

反应详情

EQUATION

反应方程式

HRID 1415546 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. washwashed with aqueous sodium bicarbonate solution
  2. dry with materialdried over potassium carbonate
  3. customAfter removal of solvent in vacuo
  4. dissolutionthe residue was dissolved in 25 ml
  5. filtrationof petroleum ether and filtered from a small amount of crystals
  6. concentrationThe filtrate was then concentrated in vacuo
  7. customchromatographed on silica gel (ether solvent)