HRID1577865

反应详情

EQUATION

反应方程式

HRID 1577865 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In a 200-ml three-necked flask equipped with dropping funnel, thermometer and reflux condenser, there were placed 4.80 g of N-ethyl-4-hydroxypiperidine, 3.23 g of pyridine and 50 ml of benzene, and 11.60 g of farnesylacetyl chloride was added dropwise under reflux. After completion of the dropping, the mixture was refluxed for a subsequent 2 hour period and then cooled. Addition of 30 ml of 20% aqueous solution of sodium hydroxide, stirring, phase separation and silica gel column chromatography of the upper layer yielded 2.4 g of N-ethyl-4-farnesylacetoxy-piperidine as a pale-yellow liquid. The product was identified by proton NMR and mass spectrometry. The proton NMR data are shown in the following.

WORKUP

后处理

  1. customIn a 200-ml three-necked flask equipped
  2. temperaturethermometer and reflux condenser
  3. additionwas added dropwise
  4. temperatureunder reflux
  5. temperatureAfter completion of the dropping, the mixture was refluxed for a subsequent 2 hour period
  6. temperaturecooled
  7. customphase separation and silica gel column chromatography of the upper layer