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

HRID 232236

반응식

HRID 232236 반응식
[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

참가 물질

4

반응물 3

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

생성물 1

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

반응 조건

온도
45 °C

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.

후처리

  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

출처 및 근거

ORD 기록
ord-caa2baf2f4e442f2908b0332d45dc432
출처 데이터셋
uspto-grants-1989_07
특허 번호
US04851531

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