Acetonitrile → N-(1-hexylpiperidin-4-yl)xanthene-9-carboxamide

HRID 370270

反応式

C(=O)([O-])[O-].[K+].[K+].I[CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH3:13].C(#N)C.Cl.[NH:18]1[CH2:23][CH2:22][CH:21]([NH:24][C:25]([CH:27]2[C:40]3[CH:39]=[CH:38][CH:37]=[CH:36][C:35]=3[O:34][C:33]3[C:28]2=[CH:29][CH:30]=[CH:31][CH:32]=3)=[O:26])[CH2:20][CH2:19]1>O>[CH2:8]([N:18]1[CH2:19][CH2:20][CH:21]([NH:24][C:25]([CH:27]2[C:28]3[CH:29]=[CH:30][CH:31]=[CH:32][C:33]=3[O:34][C:35]3[C:40]2=[CH:39][CH:38]=[CH:37][CH:36]=3)=[O:26])[CH2:22][CH2:23]1)[CH2:9][CH2:10][CH2:11][CH2:12][CH3:13]

参加物

実験手順

60 mg of potassium carbonate and 25 ml of iodohexane were successively added to 5.0 ml of acetonitrile suspension having 50 mg of N-(piperidin-4-yl)xanthene-9-carboxamide hydrochloride, followed by reflux under heating for 4 hours. After cooled to room temperature, water was added to the reaction solution, followed by extraction with ethyl acetate and drying over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure, the obtained residue was purified by preparative thin layer chromatography (Kieselgel™60F254, Art5744 produced by Merck Co.: chloroform/methanol=10/1), and 35 mg of the title compound as a white solid was obtained.

後処理

temperatureby reflux
temperatureunder heating for 4 hours
extractionfollowed by extraction with ethyl acetate
dry with materialdrying over anhydrous magnesium sulfate
distillationThe solvent was distilled off under reduced pressure
customthe obtained residue was purified by preparative thin layer chromatography (Kieselgel™60F254, Art5744 produced by Merck Co.: chloroform/methanol=10/1)

出典と根拠

ORDレコード: ord-5d9b8530ec924490abf026fab400f5d0
出典データセット: uspto-grants-2000_10
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US06140338

反応式

参加物

反応物 4

生成物 1

試薬・触媒・溶媒 1

実験手順

後処理

出典と根拠

関連ノート