Hydrogen Cyanide → 1-Amino-1-methyl-4-(4-aminobut-2-yl)cyclohexane

HRID 232236

Reaktionsgleichung

Reaktionsgleichung von HRID 232236
[CH3:1][C:2]1[CH2:7][CH2:6][CH:5]([CH:8]([CH3:12])[CH2:9][CH2:10][NH2:11])[CH2:4][CH:3]=1.S(=O)(=O)(O)O.C#[N:19]>>[NH2:19][C:2]1([CH3:1])[CH2:7][CH2:6][CH:5]([CH:8]([CH2:9][CH2:10][NH2:11])[CH3:12])[CH2:4][CH2:3]1

Komponenten

4

Edukt 3

HCID 768Hydrogen CyanideHCID 1118Sulfuric AcidHCID 13574688gamma,4-Dimethylcyclohexene-1-propan-1-amine

Produkt 1

HCID 135746931-Amino-1-methyl-4-(4-aminobut-2-yl)cyclohexaneAusbeute 90 %

Reaktionsbedingungen

Temperatur
45 °C

Versuchsvorschrift

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.

Aufarbeitung

  1. distillationthe excess hydrocyanic acid was distilled off under vacuum
  2. addition300 ml of water were then added
  3. temperaturethe mixture was heated for 3 hours
  4. temperatureto reflux
  5. customdecanted from the precipitated salt
  6. customThe phases were separated
  7. extractionthe salts and the aqueous phase were extracted twice with toluene
  8. distillationthe mixture was distilled under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-caa2baf2f4e442f2908b0332d45dc432
Quelldatensatz
uspto-grants-1989_07
Patentnummer
US04851531

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