- Synthesis method of laspeyresia pomonella sex pheromone
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The invention relates to a synthesis method of laspeyresi pomonella sex pheromone. The method comprises the steps as follows: (1) methanol is added to methyl sorbate as a raw material, and an intermediate A sorbic alcohol is obtained through 5% palladium-carbon catalytic hydrogenation reduction; (2) the intermediate A sorbitol obtained in (1) and acetic anhydride are subjected to a reaction in ethyl acetate, triethylamine and water to obtain an intermediate B sorbic acetate; (3) 6-chlorohexanol is subjected to a reaction with trimethylchlorosilane in toluene in the presence of ethyl acetate and triethylamine, after the reaction, water is added, stirring and layering are performed, and an intermediate C6-chlorohexanol trimethylsilyl ester is obtained; (4) the intermediate B sorbic acetate and the intermediate C6-chlorohexanol trimethylsilyl ester are subjected to a reaction with sodium sand in a toluene solution, then, water and sulfuric acid are dropwise added, layering and rectification are performed, and a target product E8,E10-dodecadiene-1-ol is obtained. The synthesis method has the advantages as follows: the laspeyresi pomonella sex pheromone is synthesized from available rawmaterials, the reaction route is short, and the selectivity and product yield can be increased.
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Paragraph 0030; 0035; 0036; 0039; 0044; 0045
(2019/09/17)
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- (8E, 10E) - 8,10-dodecadienol-1-ol for the preparation of
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The invention discloses a preparation method of (8E, 10E)-8, 10-dodecadienol-1-alcohol. The method comprises the steps of: reacting 6-chlorohexanol with trimethylchlorosilane in the presence of methyl tertiary butyl ether and triethylamine at 0 to 5 DEG C to obtain chloride trimethylethoxysilane; then performing the Grignard reaction on the chloride trimethylethoxysilane to obtain a Grignard agent; and reacting (2E, 4E)-2, 4-hexadiene-1-dryocrassyl acetate with the Grignard agent to obtain (8E, 10E)-8, 10-dodecadienol-1-triethoxysilane; and finally hydrolyzing the (8E, 10E)-8, 10-dodecadienol-1-triethoxysilane to obtain (8E, 10E)-8, 10-dodecadienol-1-alcohol. According to the preparation method, both the purity and the yield of hydroxy-protecting reaction product are relatively high; and the initiating success rate of the Grignard reaction is relatively high, the purity of the coupling reaction product is high.
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Paragraph 0013; 0014
(2017/08/04)
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- Zinc mediated reactions in organic synthesis: Efficient synthesis of silyl ethers under mild conditions
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General and practical method for the syn the sis of silyl ethers in the presence of zinc powder under mild conditions has been described.
- Bandgar, Babasaheb Pandurang,Chavare, Satish Navnath,Pandit, Shivaji Sandu
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p. 125 - 128
(2007/10/03)
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- Silicon-29 NMR spectra of trimethylsilylated alcohols
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29Si NMR spectra of trimethylsilyl (TMS) derivatives of 26 simple alcohols were measured under standardized conditions (i.e., in sufficiently diluted deuteriochloroform solutions). Due to association with the solvent the chemical shifts are in almost all cases larger than those reported earlier for different solutions. This observation is in agreement with the proposed mechanism of steric effects as being due to sterically controlled association with the solvent. The use of chloroform as a solvent enhances steric effects hut at the same time it can reduce small differences due to polar effects in closely related compounds. In the studied class of compounds the gross dependence of the chemical shift on polar effects is not substantially affected by the change of the solvent.
- Kvicalova, Magdalena,Cermak, Jan,Blechta, Vratislav,Schraml, Jan
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p. 816 - 820
(2007/10/03)
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- Carbofunctional silacyclobutanes 1. Synthesis of 1-(ω-hydroxyalkyl)silacyclobutanes
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A four-step synthesis of 1-(ω-hydroxyalkyl)- and 1-(4-hydroxyphenyl)silacyclobutanes was carried out. The influence of the structure of the initial compounds and the reaction conditions on the ratio of the reaction products formed was studied. The stabili
- Ushakov,Fedorova
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p. 901 - 910
(2007/10/03)
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- Process of preparing trimethylsilyloxy functionalized alkyllithium compounds
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A process for producing compounds of the formula (CH3)3 SiORLi where in R is selected from alkyl groups containing 2 to 10 carbon atoms and aryl groups containing 6 to 10 carbon atoms by reacting, in an inert atmosphere, in a hydrocarbon solvent, a haloalcohol of the formula HORX wherein R is selected from alkyl groups containing 2 to 10 carbon atoms and aryl groups containing 6 to 10 carbon atoms and X is selected from chlorine or bromine, is reacted with hexamethyldisilazane at a temperature between 20° C. and the reflux temmperature of the solvent after which the resulting product, a trimethylsilyloxyalkylhalide compound, is reacted at a temperature between 50° and 160° C., with powdered lithium metal to produce the (CH3)3 SiORLi compound.
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- An Efficient Synthesis of α,β-Unsaturated Aldehydes by a Four-Carbon Unit Extension of Grignard Reagents
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Copper-catalyzed addition of organomagnesium halides to 2-(2,2-diethoxy-ethyl)oxirane (1) affords aldol acetals 2 which upon acid treatment undergo hydrolysis and dehydration to give α,β-unsaturated aldehydes 7 with high yields.
- Cloux, Roland,Schlosser, Manfred
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p. 1470 - 1474
(2007/10/02)
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- 7- AND 8-MEMBERED OXASILACYCLOALKANES-I PREPARATION
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Some new α-trimethylsiloxy-ο-methyl(ethoxy)silyl substituted alkanes of the formula (CH3)3SiO(CH2)nSi(CH3)x=(OC2H5)3-x (x=0,1,2; n=5,6) were synthesized.These compounds are stable and can undergo base catalysed decomposition producing 1-oxa-2-sila-2,2-dis
- Chvalovsky, V.,El-Hamouly, W. S.
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p. 1195 - 1197
(2007/10/02)
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