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Potassium Iodide → HCID 21568339、化合物

HRID 1579328
ノート
印刷プレビュー

反応式

HRID 1579328 の反応式
[C:1]1([C:7]([C:15]2[CH:20]=[CH:19][C:18]([Cl:21])=[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.[C:22]([C:26]1[CH:31]=[CH:30][C:29]([C:32](=[O:37])[CH2:33][CH2:34][CH2:35]Cl)=[CH:28][CH:27]=1)([CH3:25])([CH3:24])[CH3:23].C(=O)(O)[O-].[K+].[I-].[K+]>O.C1(C)C=CC=CC=1>[ClH:21].[C:22]([C:26]1[CH:27]=[CH:28][C:29]([C:32](=[O:37])[CH2:33][CH2:34][CH2:35][N:12]2[CH2:13][CH2:14][CH:9]([C:7]([OH:8])([C:15]3[CH:16]=[CH:17][C:18]([Cl:21])=[CH:19][CH:20]=3)[C:1]3[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=3)[CH2:10][CH2:11]2)=[CH:30][CH:31]=1)([CH3:25])([CH3:24])[CH3:23]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 4875Potassium IodideHCID 516893Potassium BicarbonateHCID 27236944'-tert-Butyl-4-chlorobutyrophenoneHCID 12795120HCID 12795120、化合物

生成物 1

HCID 21568339HCID 21568339、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒
HCID 1140
Toluene
溶媒

実験手順

A mixture of 11 g (0.035 mole) of α-phenyl-α-(p-chlorophenyl)-4-piperidinemethanol, 12.5 g (0.05 mole) of 4'-tert-butyl-4-chlorobutyrophenone, 10 g of potassium bicarbonate, 0.1 g of potassium iodide, 100 ml of toluene and 10 ml of water is refluxed with stirring for about 93 hours. Upon cooling to room temperature the mixture is filtered and the toluene layer is separated. The aqueous layer is extracted with toluene. The combined organic fractions are washed with water and saturated sodium chloride solution, dried over magnesium sulfate, and filtered. To the filtrate is added an equal volume of ether followed by treatment with ethereal HCl. The resulting precipitate is collected and recrystallized from methanol-butanone to give 4'-tert-butyl-4-[4-[α-hydroxy-α-(p-chlorophenyl)benzyl]-piperidino]butyrophenone hydrochloride, M.P. 238.5°-240°C.

後処理

  1. temperatureis refluxed
  2. filtrationis filtered
  3. customthe toluene layer is separated
  4. extractionThe aqueous layer is extracted with toluene
  5. washThe combined organic fractions are washed with water and saturated sodium chloride solution
  6. dry with materialdried over magnesium sulfate
  7. filtrationfiltered
  8. additionTo the filtrate is added an equal volume of ether
  9. customThe resulting precipitate is collected
  10. customrecrystallized from methanol-butanone

出典と根拠

ORDレコード
ord-7308669c48824978b118ea29e628ebca
出典データセット
uspto-grants-1976_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03931197

反応ノート

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