- Method for preparing 1-poxlene -8-thiol
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The invention belongs to the technical field of fine chemistry, and provides a method for preparing 1-poxlene-8-thiol, wherein a-terpineol is used as a raw material, and the a-terpineol reacts with athioreagent to obtain the 1-poxlene -8-thiol, the method comprises the following steps: dissolving the a-terpineol in an organic solvent; adding the thioreagent in batches to carry out a thioreaction;the system after reaction is cooled to room temperature, the solvent is removed through rotating evaporation, and sodium hydroxide aqueous solution is slowly added until the pH value is more than orequal to 12; extracting the water phase with methyl tert-ether twice, combining the organic phase, washing with saturated brine once, drying with anhydrous sodium sulfate, concentrating, and distilling under reduced pressure to obtain the product 1-poxlene-8-thiol. The method solves the problems that in the prior art, the synthesis route of the 1-poxlene-8-thiol is complex, the lithium aluminum tetrahydrate in the raw material is expensive, the danger is high, and the prior method is not suitable for industrial production.
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Paragraph 0039-0103
(2019/06/27)
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- Synthesis process method of p-menon-1-ene-8-thiol
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The invention discloses a synthesis process method of p-menon-1-ene-8-thiol, in particular to a novel synthesis process method for obtaining p-menon-1-ene-8-thiol by using cheap synthetic perfume alpha-terpineol obtained from turpentine oil as a raw material to be reacted with thioacetic acid and then adopting LiAlH4 for reduction. The synthesis process method has the advantages that the synthesisroute is short, the process operation is simple, raw materials and reagents are easy to obtain and cheap, the first reaction cycle is shortened, the yield is high, and more importantly, the cost is greatly reduced.
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Paragraph 0017; 0019; 0020; 0022; 0023; 0025; 0026; 0028
(2019/04/26)
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- ADDITION OF H2S TO TERPENES FOR PRODUCING NOVEL MOLAR MASS REGULATORS FOR RADICAL POLYMERISATIONS
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The present invention relates to a method for producing thiols through addition of hydrogen sulfide onto at least one unsaturated terpene, where the reaction is carried out in the presence of at least one organic ion exchanger, and to the use of thiols derived from terpinolene as molar mass regulator in the polymerization of monomers.
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Page/Page column 3
(2010/02/17)
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- Simple synthetic protocols for tertiary alkyl and allyl thiols
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Convenient preparative methods for tertiary alkyl and allyl thiols are described. Accordingly, thiolesters and thiocyanates, obtained from the reaction of SN1-active halides and appropriate zinc salts, on hydrolysis and LAH reduction respectively, afford the corresponding thiols in near quantitative yields. Besides the well known p-menth-1-ene-8-thiol, p-menthane-1-thiol, p-mentha-1,8-diene-6-thiol and 2-(2-phenyl)propane thiol have been prepared.
- Gurudutt, K. N.,Rao, Sanjay,Srinivas, P.,Srinivas, S.
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p. 1169 - 1171
(2007/10/03)
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- Direct Conversion of Alcohols into Thiols
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A simple one-pot reaction between alcohols and 2,4-bis(4-methoxyphenyl)-1,3,2,4-dithiadiphosphetane 2,4-disulfide (Lawesson's reagent, LR) affords the corresponding thiols, accompanied by dehydration products, alkenes.Treatment of acyclic 1,4-diols with LR gives the 1,3-dienes. o-(Dihydroxymethyl)benzene derivatives yield the 1,3-dihydrobenzothiophenes when treated with LR.
- Nishio, Takehiko
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p. 1113 - 1118
(2007/10/02)
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- ELECTROPHILIC THIYLATION OF BICYCLIC MONOTERPENES BY HYDROGEN SULFIDE AND 1-BUTANETHIOL
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The thiylation of α,β-pinenes and camphene by hydrogen sulfide and 1-butanethiol, catalyzed by aluminum halides and alkylaluminum halides, was investigated.The regioselectivity and stereoselectivity of the reaction depend on the acidity of the catalyst.The thiylation of pinenes by hydrogen sulfide in the presence of alkylaluminum halides leads to the preferential formation of trans-pinane-2-thiol, and the catalyst with the higher acidity (aluminum bromide) promotes the menthene isomerization of the pinenes.
- Tolstikov, G. A.,Kanzafarov, F. Ya.,Dzhemilev, U. M.,Kantyukova, R. G.,Zelenova, L. M.
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p. 1799 - 1804
(2007/10/02)
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- 1-p-Menthene-8-thiol: A Powerful Impact Constituent of Grapefruit Juice (Citrus paradisi MACFAYDEN)
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1-p-Menthene-8-thiol (B) is shown to be a potent character-donating constituent of grapefruit juice, in which ir occurs at the ppb-level or below.A convenient synthesis is described for this terpene-thiol, apparently the most powerful flavor compound ever found in nature.
- Demole, Edouard,Enggist, Paul,Ohloff, Guenther
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p. 1785 - 1794
(2007/10/02)
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