反応 #483785

ord-77b2d92464384badaef3cf0ec5b4ea69

反応方程式

Cl.O.O=C1CCNCC1
4-piperidone monohydrate hydrochloride
[Al+3].[Cl-].[Cl-].[Cl-]
AlCl3
c1ccccc1
benzene
O
water
Cl.c1ccc(C2(c3ccccc3)CCNCC2)cc1
off-white solid
収率 72.0%
Cl.c1ccc(C2(c3ccccc3)CCNCC2)cc1
4,4-Diphenylpiperidine hydrochloride
収率 72.0%

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度at reflux for 4 hours
  2. 2
    ろ過filtered
  3. 3
    洗浄The solid was washed with toluene
  4. 4
    その他dried

実験手順

A mixture of 4-piperidone monohydrate hydrochloride (15.0 g, 97.6 mmol, 1.00 equiv) and AlCl3 (130 g, 976 mmol, 10.0 equiv) in anhydrous benzene (600 mL) was stirred at reflux for 4 hours. The mixture was cooled to room temperature, poured into ice (300 g) and water (50 mL), and filtered. The solid was washed with toluene and dried to afford 19.2 g (72%) of off-white solid, which was characterized spectroscopically.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06608086B2uspto-grants-2003_08