Potassium Iodide → 1-Butanone, 1-(4-fluorophenyl)-4-(4-(hydroxydiphenylmethyl)-1-piperidinyl)-, hydrochloride

HRID 1658658ノート

反応式

HRID 1658658 の反応式
[C:1]1([C:7]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)([CH:9]2[CH2:14][CH2:13][NH:12][CH2:11][CH2:10]2)[OH:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[Cl:21][CH2:22][CH2:23][CH2:24][C:25]([C:27]1[CH:32]=[CH:31][C:30]([F:33])=[CH:29][CH:28]=1)=[O:26].[I-].[K+].C(=O)(O)[O-].[Na+]>C1(C)C=CC=CC=1>[ClH:21].[F:33][C:30]1[CH:29]=[CH:28][C:27]([C:25](=[O:26])[CH2:24][CH2:23][CH2:22][N:12]2[CH2:13][CH2:14][CH:9]([C:7]([OH:8])([C:15]3[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=3)[C:1]3[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=3)[CH2:10][CH2:11]2)=[CH:32][CH:31]=1

参加物

6

反応物 4

HCID 4875Potassium IodideHCID 15723AzacyclonolHCID 197503-(4-Fluorobenzoyl)propyl chlorideHCID 516892Sodium Bicarbonate

生成物 1

HCID 2061821-Butanone, 1-(4-fluorophenyl)-4-(4-(hydroxydiphenylmethyl)-1-piperidinyl)-, hydrochloride

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A mixture of 26.73 g (0.1 mole) of α,α -diphenyl-4-piperidinemethanol, 22 g (0.11 mole) of 4-chloro-4' -fluorobutyrophenone, a trace of potassium iodide and 13.5 g (0.16 mole) of sodium bicarbonate in 500 ml of toluene was refluxed for 21/2 days. The mixture was filtered, and the filtrate was cooled. The resulting solid was converted by generally known methods to the hydrochloride salt which was recrystallized from methanol and butanone to give the desired product, M.P. 224.5°-225.5° C.

後処理

  1. filtrationThe mixture was filtered
  2. temperaturethe filtrate was cooled
  3. customwas recrystallized from methanol and butanone

出典と根拠

ORDレコード
ord-f908f56bbab342eea966ce478e33b3bd
出典データセット
uspto-grants-1976_06
特許番号
US03965257

反応ノート

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