Water → 2-Chloro-4-(3-methyl-4-methylmercapto-phenoxy)-pyridine

HRID 1262781

Reaktionsgleichung

Reaktionsgleichung von HRID 1262781
[CH3:1][C:2]1[CH:3]=[C:4]([OH:10])[CH:5]=[CH:6][C:7]=1[S:8][CH3:9].[Cl:11][C:12]1[CH:17]=[C:16]([N+]([O-])=O)[CH:15]=[CH:14][N:13]=1.C([O-])([O-])=O.[K+].[K+].O>C(#N)C>[Cl:11][C:12]1[CH:17]=[C:16]([O:10][C:4]2[CH:5]=[CH:6][C:7]([S:8][CH3:9])=[C:2]([CH3:1])[CH:3]=2)[CH:15]=[CH:14][N:13]=1

Komponenten

6

Edukt 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 183913-Methyl-4-(methylthio)phenolHCID 7351522-Chloro-4-nitropyridine

Produkt 1

HCID 130736652-Chloro-4-(3-methyl-4-methylmercapto-phenoxy)-pyridine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

A solution of 17 gm (0.1 mol) of 3-methyl-4-methylmercaptophenol and 15.9 gm (0.1 mol) of 2-chloro-4-nitropyridine in 150 ml of acetonitrile was mixed with 13.8 gm (0.1 mol) of K2CO3 and stirred for 3 hours under reflux. It was then cooled and poured into 300 ml of water. The oil which separated out was separated off and taken up in methylene chloride, and the solution was washed with dilute sodium hydroxide solution and with water. The organic solution was then dried over Na2SO4 and concentrated by evaporation. The oil which remained was crystallized from hexane.

Aufarbeitung

  1. temperatureunder reflux
  2. temperatureIt was then cooled
  3. customThe oil which separated out
  4. customwas separated off
  5. washthe solution was washed with dilute sodium hydroxide solution and with water
  6. dry with materialThe organic solution was then dried over Na2SO4
  7. concentrationconcentrated by evaporation
  8. customThe oil which remained was crystallized from hexane

Quellen und Nachweise

ORD-Eintrag
ord-1838b3c0eac4477f8df4cdf9a0d5ea63
Quelldatensatz
uspto-grants-1984_06
Patentnummer
US04453972

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