- Green synthesis method of hydroxyl citronellal
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The invention discloses a green synthesis method of hydroxyl citronellal, which comprises the following steps: (1) hydroxycitronellal. Acetonitrile, Fe (NO)3 )3 ? 9H2 O And 4 - OH-TEMPO were mixed homogeneously in the reactor and warmed up. (2) To the reactor of step (1), the reaction solution is subjected to pressure reduction to recover the crude product after the reaction, and the crude product is obtained by rectification to obtain the hydroxyl citronellal finished product. To Fe (NO), the hydroxyl citronellol is used as a raw material. 3 )3 /4 - OH-TEMPO catalytic system catalytic molecule oxidation hydroxyl citronellal to synthesize hydroxyl citronellal, and the catalytic efficiency is high. The method is high in reaction selectivity, high in yield, mild in reaction condition, high in production efficiency, simple in process and low in process cost.
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Paragraph 0007; 0012-0018
(2021/11/21)
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- Efficient green synthesis method of hydroxycitronellal
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The invention discloses an efficient green synthesis method of hydroxycitronellal. The method comprises the following steps: adding POL-PPh3, PdCl2 and anhydrous THF into a sealed container according to a mass ratio of (100: 5)-(10: 1), reacting at 25-35 DEG C overnight, filtering, removing filtrate, washing filter residues twice with ethyl acetate and ethanol respectively, and collecting solids to obtain a POL-PPh3-coated PdCl2 solid catalyst; taking 1 part by mass of a POL-PPh3-coated PdCl2 catalyst, 10-35 parts by mass of citronellal, 7-20 parts by mass of water and 500-800 parts by mass of toluene, uniformly stirring, and reacting at 180-200 DEG C for 10-24 hours to obtain a reaction solution; after the reaction liquid is cooled, filtering and separating the solid catalyst, fractionating the reaction liquid, and collecting a distillate at 257 DEG C, thereby obtaining the hydroxycitronellal. According to the method, citronellal and water are directly synthesized into hydroxycitronellal in one step under the catalysis of POL-PPh3-coated PdCl2, the method has the advantages of being environmentally friendly, low in price, high in catalytic efficiency, high in yield, mild in reaction condition, high in production efficiency, simple in process, non-toxic, harmless, free of emission of three wastes and the like, and a good foundation is laid for large-scale production of hydroxycitronellal.
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Paragraph 0013; 0027; 0030-0032; 0035; 0038-0040; 0041; ...
(2021/06/26)
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- Preparation method of citronellal hydrate
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The invention relates to a preparation method of citronellal hydrate. The method comprises the steps of citronellal oxazolidine derivative preparation, solid acid catalytic reaction, aftertreatment and the like. The purity of a citronellal hydrate product prepared by using the method provided by the invention reaches 95% or above. The method provided by the invention has the characteristics that asolid acidification catalyst is easily separated from a reactant, can be repeatedly used and cannot corrode a reactor, catalytic public hazards are reduced, and the wastewater amount is greatly reduced. By using the method provided by the invention, an environment-friendly synthesis process route is achieved.
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Paragraph 0065; 0069; 0070; 0078; 0086; 0094; 0102
(2018/04/03)
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- OXIDATION OF PRIMARY ALCOHOLS TO ALDEHYDES CATALYZED BY RUTHENIUM COMPOUNDS
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The RuCl3 and RuO2*nH2O catalyzed oxidation of alkanes, aromatic fatty acids, alcohols, citronellol and hydroxycitronellol by NaOCl was studied in the diphase system CCl4-aqueous NaOCl at pH 13-13.5.At 60 - 65 deg C, using 1-2 mole percent of catalyst and a 1.5-fold molar excess of NaOCl, primary alkanols (hexanol-1, 2-ethylhexanol-1, decanol-1, hexadecanol-1) benzyl and 3-phenylpropyl alcohols, and hydroxycitronellol are converted to the corresponding aldehydes with a selectivity of 70-90percent and a yield of over 75percent.
- Ogibin, Yu. N.,Ilovaiskii, A. I.,Nikishin, G. I.
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- NEW APPROACHES TO THE SYNTHESIS OF 7-ALKOXY- AND 7-HYDROXY-6,7-DIHYDROCITRALS
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7-Alkoxy-6,7-dihydrocitrals were obtained by the rearrangement of ethynylcarbinols in the presence of polyvanadioorganosiloxane. 7-Hydroxy-6,7-dihydrocitral was obtained by the hydration of citral 1,3-disulfonate in an acidic medium followed by alkaline decomposition of the hydration product.
- Erman, M. B.,Golovacheva, E. V.,Gulyi, S. E.,Zasetskii, D. L.,Shutikova, L. A.,et al.
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p. 219 - 221
(2007/10/02)
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- PREPARATION OF DERIVATIVES OF CITRONELLAL
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The hydrogenation of citronellal and citral, if not separated from ethereal oils, leads regioselectively to dihydrocitronellal and citronellal, respectively.The reaction of citral with (+)-ephedrin or L-aspartic acid, followed by hydrogenation and deblocking the aldehyde function, yields optically active citronellal.Reacting the aldehyde function of citronellal with diethanolamine, piperidine or morpholine, the alcohol addition to the 6,7-double bond results in 7-alkoxy substituted citronellals with acceptable yield.The formation of 7-hydroxy-6,7-dihydrocitronellal during this reaction has been proved and the effect of reaction parameters on the yield have been discussed.
- Koertvelyessy, Gyula
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p. 347 - 354
(2007/10/02)
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- Process for preparing hydroxycitronellal
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A process as described for preparing hydroxycitronellal by isomerizing certain 7-hydroxygeranylamine compound or 7-hydroxynerylamine compounds using a catalyst comprising a divalent palladium compound and a phosphine compound.
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