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Sodium Hydroxide → HCID 21105604, Verbindung

HRID 2426646
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2426646
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]([CH3:23])[C:9](=[O:22])[C:10]2[CH:15]=[CH:14][C:13]([CH:16]3[CH2:21][CH2:20][CH2:19][CH2:18][CH2:17]3)=[CH:12][CH:11]=2)=[CH:4][CH:3]=1.P([O-])([O-])([O-])=O.[Na+].[Na+].[Na+].[Br:32][CH:33]([CH2:37][CH2:38]Cl)[C:34](Br)=[O:35].[OH-].[Na+]>C(#N)C.O>[Br:32][CH:33]1[CH2:37][CH2:38][N:1]([C:2]2[CH:7]=[CH:6][C:5]([N:8]([CH3:23])[C:9](=[O:22])[C:10]3[CH:15]=[CH:14][C:13]([CH:16]4[CH2:21][CH2:20][CH2:19][CH2:18][CH2:17]4)=[CH:12][CH:11]=3)=[CH:4][CH:3]=2)[C:34]1=[O:35]
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Komponenten

7

Edukt 4

HCID 14798Sodium Hydroxide2×HCID 24243Trisodium PhosphateHCID 110327462-Bromo-4-chlorobutyryl bromideHCID 21105617HCID 21105617, Verbindung

Produkt 1

HCID 21105604HCID 21105604, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962
Water
Lösungsmittel
2×
HCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

N-(4-Aminophenyl)-4-cyclohexyl-N-methylbenzamide (3.0 g) in acetonitrile (30 ml) was mixed with trisodium phosphate (0.95 g) and, at 0° C., 2-bromo-4-chlorobutyryl bromide (2.9 g) was added. After one hour, a solution of sodium hydroxide (0.85 g) in water (10 ml) was added and the mixture was stirred vigorously at room temperature for 6 hours. The same amount of sodium hydroxide solution was then added, and stirring was continued for 48 hours. The reaction solution was diluted with water and extracted with ethyl acetate. The organic phase was dried over magnesium sulfate and concentrated. The residue was purified by chromatography on silica gel (mobile phase ethyl acetate/heptane 1:2). This resulted in the product with the molecular weight of 455.40 (C24H27BrN2O2); MS (ESI): 456 (M+H+).

Aufarbeitung

  1. stirringstirring
  2. waitwas continued for 48 hours
  3. extractionextracted with ethyl acetate
  4. dry with materialThe organic phase was dried over magnesium sulfate
  5. concentrationconcentrated
  6. customThe residue was purified by chromatography on silica gel (mobile phase ethyl acetate/heptane 1:2)
  7. customThis resulted in the product with the molecular weight of 455.40 (C24H27BrN2O2)

Quellen und Nachweise

ORD-Eintrag
ord-e86ca7d9e38543bbbfb490f8da321a12
Quelldatensatz
uspto-grants-2011_06
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07968550B2

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