Hydrogen Cyanide → 3-Cyano-3,5,5-trimethylcyclohexanone

HRID 377047

반응식

HRID 377047 반응식
[O:1]=[C:2]1[CH2:9][C:6]([CH3:8])([CH3:7])[CH2:5]C(C)=[CH:3]1.C[N+:12]1[CH:16]=[C:15]([C:17]([O-])=O)N(C)C=1.C#N>>[CH3:5][C:6]1([CH3:8])[CH2:7][C:15]([C:16]#[N:12])([CH3:17])[CH2:3][C:2](=[O:1])[CH2:9]1

참가 물질

4

반응물 3

HCID 768Hydrogen CyanideHCID 6544Isophorone2회HCID 4799511,3-Dimethylimidazolium-4-carboxylate

생성물 1

HCID 990683-Cyano-3,5,5-trimethylcyclohexanone

반응 조건

온도
150 °C

실험 절차

622 g (4.5 mol) of isophorone and 1.8 g (12.9 mmol) of 1,3-dimethylimidazolium-4-carboxylate were placed in a reaction vessel and a mixture of 207.3 g (1.5 mol) of isophorone and 81.0 g (3 mol) of hydrogen cyanide was added at 150° C. over a period of about 60 minutes. The mixture was subsequently stirred further for about 60 minutes at 150° C. After cooling, the HCN concentration was determined by titration. No free hydrocyanic acid could be detected (HCN conversion>99.9%). After addition of 2.0 g of 85% strength H3PO4, the reaction product was distilled at 0.1 hPa. This gave 486 g of 3-cyano-3,5,5-trimethylcyclohexanone (98.1% based on HCN used). The amount of distillation residue was only 3% by weight, based on isophorone used.

후처리

  1. additionwas added at 150° C. over a period of about 60 minutes
  2. temperatureAfter cooling
  3. concentrationthe HCN concentration
  4. additionAfter addition of 2.0 g of 85% strength H3PO4
  5. distillationthe reaction product was distilled at 0.1 hPa
  6. distillationThe amount of distillation residue

출처 및 근거

ORD 기록
ord-d62457d87f164db197752cd06ca6322d
출처 데이터셋
uspto-grants-2000_02
특허 번호
US06022988

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