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

HRID 232236

反応式

HRID 232236 の反応式
[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

参加物

4

反応物 3

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

生成物 1

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

反応条件

温度
45 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-caa2baf2f4e442f2908b0332d45dc432
出典データセット
uspto-grants-1989_07
特許番号
US04851531

関連ノート

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