반응 #319418

반응 방정식

amine

3-(1-methylcyclohexen-4-yl)-butylamine

sulphuric acid

hydrocyanic acid

→

1-amino-1-methyl-4-(4-aminobut-2-yl)cyclohexane

수율 90.0%

반응 조건

후처리

1. 1
   workup.DISTILLATIONthe excess hydrocyanic acid was distilled off under vacuum
2. 2
   workup.ADDITION300 ml of water were then added
3. 3
   온도the mixture was heated for 3 hours
4. 4
   온도to reflux
5. 5
   기타decanted from the precipitated salt
6. 6
   기타The phases were separated
7. 7
   추출the salts and the aqueous phase were extracted twice with toluene
8. 8
   workup.DISTILLATIONthe mixture was distilled under vacuum

실험 절차

660 g of this amine were added dropwise to 1200 g of 70% sulphuric acid at 5 to 10° C. 170 ml of hydrocyanic acid were then added dropwise at 30 to 35° C., the mixture was stirred for a further 4 hours at 45° C. and the excess hydrocyanic acid was distilled off under vacuum. 300 ml of water were then added and the mixture was heated for 3 hours to reflux, rendered alkaline with 1400 ml of 45% sodium hydroxide solution and decanted from the precipitated salt. The phases were separated, the salts and the aqueous phase were extracted twice with toluene and the mixture was distilled under vacuum. 656 g (90%) of 1-amino-1-methyl-4-(4-aminobut-2-yl)cyclohexane, b.p.10 135 to 137° C. were obtained.

출처