Potassium Carbonate → HCID 14720346, Verbindung

HRID 2352003Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2352003
[CH3:1][C:2]1[CH:7]=[C:6]([CH3:8])[CH:5]=[CH:4][C:3]=1[NH:9][CH2:10][C:11]1[CH:12]=[N:13][CH:14]=[CH:15][CH:16]=1.C(=O)([O-])[O-].[K+].[K+].[CH3:23][S:24](Cl)(=[O:26])=[O:25]>ClCCl>[CH3:1][C:2]1[CH:7]=[C:6]([CH3:8])[CH:5]=[CH:4][C:3]=1[N:9]([CH2:10][C:11]1[CH:12]=[N:13][CH:14]=[CH:15][CH:16]=1)[S:24]([CH3:23])(=[O:26])=[O:25]

Komponenten

5

Edukt 3

HCID 11430Potassium CarbonateHCID 31297Methanesulfonyl chlorideHCID 14720345N-(2,4-Dimethylphenyl)-3-pyridinemethanamine

Produkt 1

HCID 14720346HCID 14720346, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

A 4.2 g. portion of 3-(2,4-dimethylphenylaminomethyl)pyridine was dissolved in 20 ml. of dichloromethane and 4.1 g. of potassium carbonate and 2.5 ml. of methanesulfonyl chloride were added. The mixture was stirred over the week-end under reflux, and was then extracted with 20 ml. of aqueous sodium bicarbonate. The organic phase was dried and evaporated under vacuum. The residue was dissolved in diethyl ether and the solution was separated from insolubles and evaporated under vacuum. The oil was dissolved in chloroform and chromatographed over silica gel, eluting with chloroform:ethyl acetate to obtain 2.5 g. of the desired product, m.p. 62°-65°.

Aufarbeitung

  1. temperatureunder reflux
  2. extractionwas then extracted with 20 ml
  3. customThe organic phase was dried
  4. customevaporated under vacuum
  5. dissolutionThe residue was dissolved in diethyl ether
  6. customthe solution was separated from insolubles
  7. customevaporated under vacuum
  8. dissolutionThe oil was dissolved in chloroform
  9. customchromatographed over silica gel
  10. washeluting with chloroform
  11. customethyl acetate to obtain 2.5 g

Quellen und Nachweise

ORD-Eintrag
ord-c171eccab5be47df84d51ba3e43722bc
Quelldatensatz
uspto-grants-1989_10
Patentnummer
US04874775

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