反応 #55011

ord-d57b5d7ea41b4259acc2bd37a7ee7e13

反応方程式

Cc1ccc(S(=O)(=O)O)cc1
4-methylbenzenesulfonic acid
CCOC(=O)N1CCC(=O)CC1
ethyl 4-oxo-1-piperidinecarboxylate
Nc1ccc(Cl)cc1
4-chlorobenzeneamine
Cc1ccccc1
methylbenzene
CCOC(=O)N1CCC(=Nc2ccc(Cl)cc2)CC1
ethyl 4-[(4-chlorophenyl)imino]-1-piperidine-carboxylate

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度refluxed for 7 hours
  2. 2
    その他(The reaction vessel is provided with
  3. 3
    温度a reflux-condensor
  4. 4
    その他The methylbenzene is evaporated
  5. 5
    workup.DISTILLATIONthe oily residue is distilled in vacuo

実験手順

A mixture of 171.2 parts of ethyl 4-oxo-1-piperidinecarboxylate, 159.5 parts of 4-chlorobenzeneamine, 1520 parts of anhydrous methylbenzene and a few crystals of 4-methylbenzenesulfonic acid is stirred and refluxed for 7 hours. (The reaction vessel is provided with a reflux-condensor and water-separator). The methylbenzene is evaporated and the oily residue is distilled in vacuo, yielding 192 parts of oily ethyl 4-[(4-chlorophenyl)imino]-1-piperidine-carboxylate; bp. 171°-176° C. at 0.4 mm. pressure.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04151286uspto-grants-1979_04