反応 #747094

反応方程式

hydrogen peroxide

1-(4-aminophenyl)-N,N,N-trimethylpyrrolidin-3-aminium chloride hydrochloride

3-amino-2-chloro-6-methylphenol hydrochloride

ammonium hydroxide

→

1-(4-{[2-amino-3-chloro-5-methyl-4-oxocyclohexa-2,5-dien-1-ylidene]amino}phenyl)-N,N,N-trimethylpyrrolidin-3-aminium chloride

収率 39.1%

溶媒

water

water

反応条件

後処理

1. 1
   workup.WAITThe mixture is left
2. 2
   ろ過The precipitate is filtered off
3. 3
   洗浄rinsed with acetone

実験手順

292.5 mg of 1-(4-aminophenyl)-N,N,N-trimethylpyrrolidin-3-aminium chloride hydrochloride and 194.1 mg of 3-amino-2-chloro-6-methylphenol hydrochloride are weighed out in a flask, 1 ml of water is added and the pH is adjusted to 9.5 with 20% ammonium hydroxide in water. 1.1 ml of 30% aqueous hydrogen peroxide solution are added dropwise. The mixture is left stirring for 24 hours. The precipitate is filtered off and rinsed with acetone. 80 mg of 1-(4-{[2-amino-3-chloro-5-methyl-4-oxocyclohexa-2,5-dien-1-ylidene]amino}phenyl)-N,N,N-trimethylpyrrolidin-3-aminium chloride (1t) are thus obtained.

出典