HCID 178418395, Verbindung → HCID 178527778, Verbindung

HRID 1589712

Reaktionsgleichung

Reaktionsgleichung von HRID 1589712
CCCCCCCCCCCCCCCCC=C.[S:19][Cl:20].[SH:21][C:22]1[S:23][C:24]2[CH:30]=[CH:29][CH:28]=[CH:27][C:25]=2[N:26]=1>CCCCCCCC[N+](CCCCCCCC)(CCCCCCCC)C.[Cl-].C1(C)C=CC=CC=1>[S:19][Cl:20].[SH:21][C:22]1[S:23][C:24]2[CH:30]=[CH:29][CH:28]=[CH:27][C:25]=2[N:26]=1

Komponenten

5

Edukt 2

HCID 178418395HCID 178418395, VerbindungHCID 178443003HCID 178443003, Verbindung

Produkt 1

HCID 178527778HCID 178527778, VerbindungAusbeute 397,2 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 21218Trioctylmethylammonium chlorideKatalysatorHCID 1140TolueneLösungsmittel

Versuchsvorschrift

278.4 gm of the product of Example 1 (0.4 mol.), 133.8 gm of 2-mercaptobenzothiazole (0.8 mol.), 8 gm of Aliquat 336 (phase transfer catalyst obtained from Aldrich Chemical Company: tricaprylylmethyl ammonium chloride), 200 ml caustic solution (32 gm sodium hydroxide dissolved in 200 ml water), and 400 ml toluene were mixed in a 2-liter reactor. The reactants were stirred under reflux for six hours, and then cooled to ambient temperature. The aqueous phase was separated, and the organic phase was twice washed with 400 ml of water. Thereafter, toluene was removed by vacuum distillation leaving a dark fluid as the desired product (373 gm). It was further purified by hot filtration through Super-Cel.

Aufarbeitung

  1. temperatureunder reflux for six hours
  2. customThe aqueous phase was separated
  3. washthe organic phase was twice washed with 400 ml of water
  4. customThereafter, toluene was removed by vacuum distillation

Quellen und Nachweise

ORD-Eintrag
ord-6fe259680bc6441d8d271f5006828699
Quelldatensatz
uspto-grants-1993_04
Patentnummer
US05199960

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