반응 #218491

반응 방정식

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

용매

ethanol

water

반응 조건

후처리

1. 1
   온도heat the mixture
2. 2
   온도under reflux for 2 hours
3. 3
   온도to cool
4. 4
   기타Collect the precipitate
5. 5
   기타formed by filtration
6. 6
   기타dry under high vacuum

실험 절차

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).

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