Hydrochloric Acid → HCID 54428804, Verbindung

HRID 341735

Reaktionsgleichung

Reaktionsgleichung von HRID 341735
N([O-])=O.[Na+].[Cl:5][C:6]1[C:12]([CH3:13])=[CH:11][CH:10]=[C:9]([Cl:14])[C:7]=1N.Cl.[CH3:16][S:17]SC>O.C(O)(=O)C.[Cu]>[Cl:5][C:6]1[C:7]([S:17][CH3:16])=[C:9]([Cl:14])[CH:10]=[CH:11][C:12]=1[CH3:13]

Komponenten

8

Edukt 4

HCID 313Hydrochloric AcidHCID 12232Dimethyl DisulfideHCID 1165292,6-Dichloro-3-methylanilineHCID 23668193Sodium Nitrite

Produkt 1

HCID 54428804HCID 54428804, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 23978CopperKatalysatorHCID 176Acetic AcidLösungsmittel2×HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

A solution of sodium nitrite (12.0 g) in water was added to a stirred suspension of 2,6-dichloro-3-methylaniline (30.0 g) in a mixture of glacial acetic acid and concentrated hydrochloric acid. While maintaining the temperature below 10° C. The mixture was stirred at 0° C. for three quarters of an hour then added to a mixture of dimethyl disulphide (20 ml) and copper powder (0.25 g) in glacial acetic acid. The mixture was stirred for 4 hours and extracted with ether. The organic layer was washed with aqueous sodium carbonate (2M), water, dried (Na2SO4) and filtered. The filtrate was evaporated to dryness to give 2,4-dichloro-3-(methylsulphenyl)toluene (27.2 g) as a red liquid NMR (CDCl3) 2.4(s,3H), 2.45(s,3H), 7.15(d,1H), 7.3(d,1H).

Aufarbeitung

  1. temperatureWhile maintaining the temperature below 10° C
  2. stirringThe mixture was stirred for 4 hours
  3. extractionextracted with ether
  4. washThe organic layer was washed with aqueous sodium carbonate (2M), water
  5. dry with materialdried (Na2SO4)
  6. filtrationfiltered
  7. customThe filtrate was evaporated to dryness

Quellen und Nachweise

ORD-Eintrag
ord-b8985a846b5a4156bb3bc733b0afee4a
Quelldatensatz
uspto-grants-1999_01
Patentnummer
US05856274

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