反応 #56405
ord-69afb760ce334456b0c8437bc4ff6a35
反応方程式
4-methylbenzenesulfonic acid
ethyl 4-oxo-1-piperidinecarboxylate
4-chlorobenzenamine
methylbenzene
→
ethyl 4-[(4-chlorophenyl)imino]-1-piperidinecarboxylate
反応物
試薬
なし
溶媒
反応条件
詳細条件
See reaction.notes.procedure_details.
後処理
- 1温度refluxed for 7 hours
- 2その他(The reaction vessel is provided with
- 3温度a reflux-condensor
- 4その他The methylbenzene is evaporated
- 5workup.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-chlorobenzenamine, 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-piperidinecarboxylate; bp. 171°-176° C. at 0.4 mm. pressure.