Reaktionsgleichung
[OH-].[CH3:2][N+:3]1[C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=2[S:5][C:4]=1SCCCS(O)(=O)=O.Cl.Cl.[NH2:22][C:23]1[CH:31]=[CH:30][C:26]2[NH:27][N:28]=[N:29][C:25]=2[CH:24]=1.C([O-])(=O)C.[Na+]>O>[CH3:2][N:3]1[C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=2[S:5](=[N:22][C:23]2[CH:31]=[CH:30][C:26]3[NH:27][N:28]=[N:29][C:25]=3[CH:24]=2)[CH2:4]1Komponenten
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 50 °C
Versuchsvorschrift
175 g of anhydrous 3-methyl-2-(3-sulfopropylthio) benzothiazolium hydroxide was added to a mixture of 100 g of 5-aminobenzotriazole di-hydrochloride, 120 g of sodium acetate and 1000 ml of water under heating at 50° C with stirring in a 2000 ml flask. After stirring for 1 hour at 85° C the mixture was cooled (15° C) with water. The precipitate formed was collected by filtration, washed with water and then with acetonitrile to yield 135 g of crystals. These crystals were dissolved by heating (90° C) in 350 ml of dimethylformamide and the solution was treated with active carbon and filtered. By addition of 1400 ml of acetonitrile to the filtrate, crystals were formed. The crystals were collected to yield 121 g of the desired compound. The melting point was 240.5° C.
Aufarbeitung
- stirringAfter stirring for 1 hour at 85° C the mixture
- customThe precipitate formed
- filtrationwas collected by filtration
- washwashed with water
Quellen und Nachweise
- ORD-Eintrag
- ord-83e9387fa1c541aeaaebcb2cb3c4802e
- Quelldatensatz
- uspto-grants-1978_06
- Patentnummer
- US04095984
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