HRID2412937

反应详情

EQUATION

反应方程式

HRID 2412937 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 1,1-dimethylethyl 1-[(4-methoxyphenyl)methyl]-4-piperidinylcarbamate (0.02 mole) and trifluoroacetic acid (0.01 mole) in 50 ml. of methylene chloride was refluxed for a 3 hr. period. Additional trifluoroacetic acid (0.08 mole) was added and reflux continued for an additional 30 minutes. The crude solution was evaporated in vacuo, residual material dissolved in water and the aqueous phase washed with ether and then made basic with 50% sodium hydroxide. Extraction of the basified solution with chloroform, drying of the chloroform extracts, and removal of the solvent afforded 4-amino-1-[(4-methoxyphenyl)methyl]piperidine in nearly quantitative yield.

WORKUP

后处理

  1. temperaturereflux
  2. customThe crude solution was evaporated in vacuo, residual material
  3. dissolutiondissolved in water
  4. washthe aqueous phase washed with ether
  5. extractionExtraction of the basified solution with chloroform
  6. dry with materialdrying of the chloroform
  7. customremoval of the solvent