Reaktion #218491

Reaktionsgleichung

2-(4-chloro-2-nitro-phenylamino)-5-methyl-thiophene-3-carbonitrile

tin(II)chloride

hydrochloric acid water

→

7-chloro-2-methyl-4H-3-thia-4,9-diaza-benzo[f]azulen-10-ylamine hydrochloride

Lösungsmittel

ethanol

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturheat the mixture
2. 2
   Temperaturunder reflux for 2 hours
3. 3
   Temperaturto cool
4. 4
   SonstigeCollect the precipitate
5. 5
   Sonstigeformed by filtration
6. 6
   Sonstigedry under high vacuum

Vorschrift

Suspend 2-(4-chloro-2-nitro-phenylamino)-5-methyl-thiophene-3-carbonitrile (2.92 g) in ethanol (40 ml), add anhydrous tin(II)chloride(5 g,) in 1:1 concentrated hydrochloric acid/water (32 ml) and heat the mixture under reflux for 2 hours. Dilute the mixture with water and allow to cool. Collect the precipitate formed by filtration and dry under high vacuum to give 7-chloro-2-methyl-4H-3-thia-4,9-diaza-benzo[f]azulen-10-ylamine hydrochloride as a yellow solid (3.3 g, 90%): mass Spectrum (FIA) 264/266 (M+1).

Quelle