- Preparation method of hexamethyl indane alcohol
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The invention discloses a preparation method of hexamethyl indane alcohol. The method comprises the following steps: reacting 1, 1, 2, 3, 3-pentamethyl indane with allyl alcohol under the action of acatalyst, and carrying out continuous rectification to separate the product. The used catalyst is a supported Ru catalyst and is prepared from a Ru precursor, a ligand, a cocatalyst and a carrier. Thesupported Ru catalyst has the main advantages that hexamethyl indane alcohol is prepared through reaction of 1, 1, 2, 3, 3-pentamethyl indane and allyl alcohol, and the supported Ru catalyst is highin activity, good in selectivity, not prone to loss, easy to operate and good in economic benefit.
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Paragraph 0058-0072
(2020/06/16)
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- Method for preparing galaxolide under catalysis of superfine aluminum trichloride
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The invention relates to a method for preparing galaxolide under catalysis of superfine aluminum trichloride. The method is characterized by comprising the following steps: 1, adding pentamethyl indanand anhydrous aluminum trichloride with particle size of 5 meshes or blow to a solvent, and cooling the solution to subzero 30-subzero 20 DEG C, wherein the mass ratio of the pentamethyl indan to anhydrous aluminum trichloride is (1.5-2):1; 2, dropwise adding propylene oxide to dissolve in the solution in the solvent during stirring, and conducting a reaction at subzero 30-subzero 5 DEG C for 1-2h to produce hexamethyl indanol, wherein the mass ratio of the propylene oxide to pentamethyl indan is (0.3-0.5):1; 3, continuously adding a deactivating agent and formaldehyde or formaldehyde equivalents, heating the mixture to 5-65 DEG C to react for 0.5-4 h to produce galaxolide, wherein the molar ratio of the deactivating agent, the formaldehyde or formaldehyde equivalents to the pentamethylindan is (1-2):1 and (0.5-1):1; and 4, performing purification. The method has the advantages as follows: aluminum trichloride powder with superfine particle size is used, the raw material conversionrate and product yield are significantly increased, the reaction time is shortened, the reaction has good reproducibility, energy is saved, production efficiency is improved, and the production cost is reduced.
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Paragraph 0015-0020
(2019/12/25)
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- Process for preparing isochroman compounds
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High-purity isochroman compounds can be obtained in high yields according to a simple and economical process for preparing isochroman compounds, comprising the step of adding an aquesous solution of formaldehyde having a concentration of 40 to 70 wt. % to a complex of an arylalkanol represented by the following general formula (II) with a Friedel-Crafts catalyst to cyclize the arylalkanol: STR1 wherein R1 and R2 each stands for a hydrogen atom, a lower alkyl group or a lower alkoxyl group, or alternatively R1 and R2 are respectively bonded to adjacent carbon atoms with mutual bonding of R1 and R2 together with the carbon atoms respectively bonded to R1 and R2 to form a benzene ring, a naphthalene ring, or a C5 or C6 cycloalkane or cycloalkene which may have 1 to 6 lower alkyl groups; and R3 stands for a hydrogen atom or a lower alkyl group.
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- Preparation of beta-aryl alcohols
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β-Aryl alcohols for the general forumla I STR1 where R1, R2 and R3 are identical or different and each is hydrogen, C1 -C20 -alkyl, C5 -C7 -cycloalkyl, aryl, C7 -C12 -aralkyl or C7 -C12 -alkaryl, n is 0, 1, 2, 3 or 4, or where two adjacent R1 's are linked to form a 5- or 6-membered ring, are prepared by reacting an aromatic of the formula II STR2 with an alkylene oxide of the formula III STR3 where R1, R2 and R3 have the abovementioned meanings, in the presence of a Friedel-Crafts catalyst, by carrying out the reaction in the presence of a titanium(IV) alcoholate at from -20° to +40° C. in the presence or absence of a solvent.
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- Process for the production of compounds useful in perfumery
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Process for producing compounds useful in perfumery including isochromans and acylated indane hydrocarbons with an alkylene oxide or with a lower acyl halide in the presence of a hydrocarbon or hydrocarbon mixture containing C5 to C10 alkanes at a temperature of from -20° C. up to -5° C. In the case of forming isochromans, the resulting alcohol is reacted, in situ, with a lower alkanol and a formaldehyde precursor at temperatures of from 20° C. up to 80° C.
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