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

HRID 440130

Reaktionsgleichung

Reaktionsgleichung von HRID 440130
[O:1]=[C:2]1[CH2:9][C:6]([CH3:8])([CH3:7])[CH2:5][C:4]([CH3:10])=[CH:3]1.[CH:11]#[N:12].OP(O)(O)=O>COC(=O)[O-].C[N+](C)(C)C>[O:1]=[C:2]1[CH2:9][C:6]([CH3:8])([CH3:7])[CH2:5][C:4]([CH3:10])=[CH:3]1.[C:11]([C:4]1([CH3:10])[CH2:5][C:6]([CH3:8])([CH3:7])[CH2:9][C:2](=[O:1])[CH2:3]1)#[N:12]

Komponenten

6

Edukt 3

HCID 768Hydrogen Cyanide2×HCID 1004Phosphoric AcidHCID 6544Isophorone2×

Produkt 2

HCID 6544IsophoroneAusbeute 99 %HCID 990683-Cyano-3,5,5-trimethylcyclohexanoneAusbeute 128,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 11804927Tetramethylammonium Methyl CarbonateKatalysator

Versuchsvorschrift

In reaction apparatus equipped with a stirrer, condenser, thermometer and dripping funnel there are placed 622 g (4.5 mol) of isophorone and 4.47 g (30 mmol) of tetramethylammonium methylcarbonate. Over a period of 60 min there are added, at 120° C., 288.3 g of a mixture of isophorone and hydrocyanic acid (3 mol of HCN, 1.5mol Of isophorone). When all of said mixture has been added, the HCN concentration is 20 ppm. 3.5g of 85% strength H3PO4 are then added and the mixture is distilled at 0.1 mbar. There are obtained 426.6g of isophorone (99% based on converted isophorone) and 476.8 g of 3-cyano-3,5,5-trimethylcyclohexanone (96.2% based on HCN used).

Aufarbeitung

  1. customIn reaction apparatus
  2. customequipped with a stirrer, condenser
  3. additionOver a period of 60 min there are added, at 120° C.
  4. additionWhen all of said mixture has been added
  5. distillationthe mixture is distilled at 0.1 mbar

Quellen und Nachweise

ORD-Eintrag
ord-fd52e61b9c3d41b28dd9e5a4f35503c9
Quelldatensatz
uspto-grants-1996_05
Patentnummer
US05516928

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