Heptanal

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Heptanal or heptanaldehyde is an alkyl aldehyde. It is a colourless liquid with a strong fruity odor, which is used as precursor to components in perfumes and lubricants.[1]

Production

The formation of heptanal in the fractional distillation of castor oil[2] was already described in 1878. The large-scale production is based on the pyrolytic cleavage of ricinoleic acid[3] (Arkema method) and on the hydroformylation of 1-hexene with rhodium 2-ethylhexanoate as a catalyst upon addition of some 2-ethylhexanoic acid (Oxea method):[1][4]

Hydroformylation of 1-Hexene

Heptanal naturally occurs in the essential oils of ylang-ylang (Cananga odorata), clary sage (Salvia sclarea), lemon (Citrus x limon), bitter orange (Citrus x aurantium), rose (Rosa) and hyacinth (Hyacinthus).[5]

Properties

Heptanal is a flammable, slightly volatile colorless liquid of pervasive fruity to oily-greasy odor,[6] which is miscible with alcohols[5] and practically insoluble in water.[7] Because of its sensitivity to oxidation, heptanal is filled under nitrogen and stabilized with 100 ppm hydroquinone.[8]

Heptanal forms flammable vapor-air mixtures. The compound has a flash point of 39.5 °C.[7] The explosion range is between 1.1% by volume as the lower explosion limit (LEL) and 5.2% by volume as the upper explosion limit.[7] Its ignition temperature is 205 °C.[7]

Uses

Heptanal can be used for the production of 1-heptanol via hydrogenation:

Synthese von 1-Heptanol

The oxidation of heptanal with oxygen in the presence of a rhodium catalysts leads at 50 °C to heptanoic acid in 95% yield.[9] Heptanal reacts with benzaldehyde in a Knoevenagel reaction under basic catalysis with high yield and selectivity (> 90%) to jasminaldehyde,[10][1] which is mostly used in fragrances for its jasmine-like aroma as a cis/trans isomer mixture.[11]

α-pentylcinnamal (jasminal) by aldol condensation of benzaldehyde with heptanal

A by-product of the given reaction is the unpleasant rancid smelling (Z)-2-pentyl-2-nonenal.[12] Nevertheless, heptanal can be converted into (Z)-2-pentyl-2-nonenal virtually quantitatively in the presence of aqueous boric acid upon azeotropic removal of water.[13]

2-Pentyl-2-nonenal by self-condensation of heptanal

Full hydrogenation provides the branched primary alcohol 2-pentylnonan-1-ol, also accessible from the Guerbet reaction from heptanol.[14]

References

  1. a b c Template:Ullmann
  2. F. Krafft, Distillation of castor oil, under reduced pressure, Analyst, 3, 329a (1878).
  3. A. Chauvel, G. Lefebvre, Petrochemical Processes: Technical and Economic Characteristics, vol. 2, p. 277, Editions Technip, Paris, 1989, Template:ISBN.
  4. A. Fischbach et al on behalf of Oxea Deutschland GmbH (20 May 2009). Verfahren zur Herstellung von Aldehyden, German patent DE 102007053385.
  5. a b G. A. Burdock, Fenaroli's Handbook of Flavor Ingredients, Fifth Edition, 2005, CRC Press, Boca Raton, Fl., Template:ISBN.
  6. Script error: No such module "Citation/CS1".
  7. a b c d Record in the GESTIS Substance Database of the Institute for Occupational Safety and HealthScript error: No such module "TemplatePar". Script error: No such module "TemplatePar".
  8. Acros Organics (rev. 19 Nov 2012). Heptaldehyde, stabilized (safety data sheet).
  9. H. Springer and P. Lappe, on behalf of Celanese Chem Europe GmbH (3 May 2001). Verfahren zur Herstellung aliphatischer Carbonsäuren aus Aldehyden, German patent DE 10010771.
  10. Script error: No such module "Citation/CS1".
  11. alpha-Amylzimtaldehyd (rev. 4 Aug 2000) at the Riechstofflexikon [Odorant Dictionary], vol. A.
  12. J. M. Hornback, Organic Chemistry, 2nd edition, p. 886, Thomson Brooks/Cole, 2006, Template:ISBN.
  13. Script error: No such module "Citation/CS1".
  14. G.H. Knothe: Lipid Chemistry, Guerbet Compounds Template:Webarchive, AOCS Lipid Library, 22 December 2011.