2-Chloro-6-methylaniline → HCID 178424119, Verbindung

HRID 1388503

Reaktionsgleichung

Reaktionsgleichung von HRID 1388503
O(CC(C)C)[C:2]([S-:4])=[S:3].[K+].Cl[C:11]1[CH:17]=[CH:16][CH:15]=[C:14]([CH3:18])[C:12]=1[NH2:13].C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[CH3:18][C:14]1[C:12]2[N:13]=[C:2]([SH:4])[S:3][C:11]=2[CH:17]=[CH:16][CH:15]=1

Komponenten

5

Edukt 3

HCID 68972-Chloro-6-methylanilineHCID 11430Potassium CarbonateHCID 23675782Potassium isobutylxanthate

Produkt 1

HCID 178424119HCID 178424119, VerbindungAusbeute 95 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel2×

Versuchsvorschrift

A solution of 250 g of potassium isobutyl xanthate (about 90% pure) in 400 ml of dimethylformamide is added dropwise to a mixture of 141.5 g of 2-chloro-6-methylaniline and 276 g of potassium carbonate in 1 liter of dimethylformamide at 150° C. in the course of one hour, under a nitrogen atmosphere. The reaction mixture is stirred for about a further 26 hours, whilst cooling intensively. The batch is cooled, freed from salt and then concentrated to dryness. The residue is taken up in 400 ml of water and the mixture is acidified. The 4-methyl-2-mercaptobenzothiazole which precipitates is filtered off, washed with water and dried. 172 g (95% of theory) of 4-methyl-2-mercaptobenzothiazole of melting point 188°-190° C. are obtained.

Aufarbeitung

  1. temperaturewhilst cooling intensively
  2. temperatureThe batch is cooled
  3. concentrationconcentrated to dryness
  4. customThe 4-methyl-2-mercaptobenzothiazole which precipitates
  5. filtrationis filtered off
  6. washwashed with water
  7. customdried

Quellen und Nachweise

ORD-Eintrag
ord-9b06297c1bab419290378df2fad8c280
Quelldatensatz
uspto-grants-1984_02
Patentnummer
US04431813

Verknüpfte Notizen

Wird geladen…