• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    Inclusion complexes of cyclodextrins and strong inorganic oxy-acids are stable and crystalline and may be stored. Such complexes may be prepared whilst inhibiting or at least in part avoiding hydrolysis and/or decomposition of the cyclodextrin providing appropriate reaction conditions of for example temperature and acid concentration are selected. Preferred strong inorganic oxy-acids include phosphoric, sulfuric and nitric acid.
    公开号:SU1269738A3
    申请号:SU813415204
    申请日:1981-10-16
    公开日:1986-11-07
    发明作者:Сейтли Йожеф；Будаи Жужанна；Пап Габриелла；Керекеш Андраш
    申请人:Хиноин Дьедьсер Еш Ведьесети Термекек Дьяра Рт (Фирма)；
    IPC主号:
    专利说明:

    1 The invention relates to a process for the preparation of inclusion complexes of cyclodextrins and strong inorganic acids. The resulting complexes can be used for analytical purposes, for internal buffering, for introducing acid into anhydrous media, for exchange or for introducing various radicals, as well as catalysts. The quenching capacity of quenching powders can be increased many times over with the addition of 5 to 0% cyclodextrin acid complex to them. The purpose of the invention is to obtain a stable product during storage. Example 1.50 g of crystalline p-cyclodextrin with heterogenous grinding is homogenized in a mortar with 50 ml of 40% aqueous phosphoric acid solution, which is pre-cooled to O C (at a ratio of 1 ml of acids per 1 g of cyclodextrin). The resulting crystals are filtered on a No. 63 glass filter, then dried in an oven at 60 ° C. The resulting product is an inclusion complex of / -cyclodextrin-phosphoric acid. 53 g of white crystalline material are obtained. The content of phosphoric acid in the resulting material is 7.1 g according to the method of alkalimetric determination. The product is crystalline based on a powder chart after X-ray diffraction, thermo-analytical studies show the structure of the complex. The insertion coefficient is 1 mol / 1 mol. The product can be stored at room temperature for more than 6 months, at 40 ° C for more than 1 month. at 60 ° C for 3 weeks. without color change and without decomposition. At 80 ° C, the material becomes slightly discolored after two weeks. Example2. 40 g of crista; hlicic (} -cyclodextrin is homogenized for 5 min with intensive trituration in a mortar with 10 ml of 40% phosphoric acid solution, which is pre-cooled to 0 C, at a ratio of 0.25 ml of acid to 1 g of cyclodextrin, then dried in a drier at 60 C. 44 g of the inclusion complex and α-cyclodextrin-phosphoric acid are obtained. The content of phosphoric acid in the product is 10% by weight, the embedding ratio is 1.4 mol / mol. product is similar to that shown in example 1. Sample. lOrJ-cyclodextrin is homogenized with intensive rubbing in a mortar from 10 ml of a 70% phosphoric acid solution at a temperature of 0 ° C, filtered, then dried in a drying cabinet at 50 ° C. 1.5 g of an α-cyclodextrin-phosphoric acid inclusion complex are obtained, where the acid content is 9, The 5% and embedding ratio is 1.4 mol / mol. The properties of the product are the same as in Example 1. Example 4. SUBL-cyclodextrin is homogenized in a grating mortar with 2.5 ml of a 30% phosphoric acid solution at a temperature of 0 ° C, then dried in an oven at 60 ° s 10.8 g of a d-complex of cyclodextrin-phosphoric acid are obtained, where the content of phosphoric acid is 7.5%, the incorporation factor is 0.83 mol / mol. Product properties are similar to those shown in example 1. Example5. The desired product is prepared as described in Example 1, but instead of phosphoric acid, a 33% solution of sulfuric acid is used. 47.5 g of a white crystalline inclusion complex, 5-cyclodextrin-sulfuric acid, are obtained. The content of sulfuric acid in the product is 8.2% by the method of alkalimetric determination (with potassium hydroxide). The insertion factor is 1.1 mol of sulfuric acid / mol of p-cyclodextrin. Crystalline complex based on powder diargamum is stable by thermoanalysis. Example South-cyclodextrin is homogenized in a mortar with 2.6 ml of a 60% aqueous solution (0.26 ml of acid per 1 g of cyclodextrin sulfuric acid, which is pre-cooled to -5 ° C, then the resulting product is dried in a vacuum dryer at 50 ° C. 11.8 g of the inclusion complex J-cyclodextrin-sulfuric acid are obtained, where the acid content is 1-5% and the incorporation factor is 2.5 mol / mol.
    Example. 10 r “; -cyclodextrin homogenized with 10 ml of 32% sulfuric acid solution, the resulting product is filtered, then dried in a vacuum desiccator at room temperature (25 ° C). 6.5 g of the oi-cyclodextrin sulfuric acid inclusion complex are obtained. The content of sulfuric acid in the product is 4.5%, the embedding ratio is 0.5 mol / mol.
    Product properties are similar to those in Example 1,
    For example, 106-cyclodextrin is homogenized with 3 ml of a 65% solution of nitric acid (0.3 ml of acid per 1 g of cyclodextrin) at -5 ° C and the resulting cypjaT product in a vacuum desiccator at room temperature. 10.8 g of the oL-cyclodextrin-nitric acid inclusion complex are obtained, where the nitric acid content is 4.1% and the incorporation factor is 0.7 mol / mol. The properties of the product are the same as in Example I.
    PRI me R 9. Get the target product according to example 1, but using instead of phosphoric acid, a 55% solution of nitric acid. 35 g of a white crystalline p-cyclodextrin-nitric acid inclusion complex are obtained. The content of nitric acid in the complex is 5.7% embedding ratio 1.2 mol / mol.
    Stability: a decrease in the content of nitric acid after 2 weeks at room temperature or after 4 days at 40 ° C in a vacuum of less than 10%.
    Example 10. 20 g of p-cyclodextrin and 10 ml of a 20% aqueous solution of nitric acid (0.5 ml of acid per 1 g of cyclodextrin) are rapidly stirred at, filtered in a cold state, and dried in a vacuum desiccator at room temperature over solid hydroxide Kali. 12 g of the jb-cyclodextrin-nitric acid inclusion complex are obtained, where the nitric acid content is 2.8% and the incorporation factor is 0.55 mol / mol.
    697384
    The properties of pro1. Ukta are similar to those shown in the example.
    Example II 40 g / 3 -cyclodextrin is mixed in a mortar with 1-0 ml of 5 85% phosphoric acid solution at (o, 25 ml of acid per 1 g of cyclodextrin), then the mixture is dried in a vacuum drying cabinet, at 80 C. As a result Komp10 leke of f-cyclodextrin and phosphoric acid B is obtained as a white powder. The content of phosphoric acid in the complex is 17%, the water content is 6%. Product properties are similar to those shown in 15 example 1.
    EXAMPLE 12 A pellet product is obtained in the same manner as in Example 11, but instead of phosphoric acid, 10 ml of a 75% aqueous solution of sulfuric acid is taken. The result is a complex of ft-cyclodextrin and sulfuric acid with a sulfuric acid content of 9.5 and water of 5%. Product properties are similar to those shown in Example 1, 25 Example13. The desired product is obtained in the same manner as in Example 11, but instead of phosphoric acid, 12.5 ml of 30% sulfuric acid are taken. As a result, a complex is obtained including 30 -cyclodextrin and sulfuric acid, you with a content of sulfuric acid 6 and water 6%. Product properties are similar to those shown in example 1,
    35 Example14. UOg of a mixture of cyclodextrins and linear dextrins (obtained by drying in a spray dryer an enzymatic broth used to obtain
    40 cyclodextrins containing 50%
    fl-cyclodextrin, 7% ot, α-cyclodextrin, 5% y-cyclodextrin and 38% linear dextrins, are mixed in the same manner as in the example AND
    45, 25 ml of a 30% phosphoric acid solution and dried in a vacuum drying cabinet at 60 C. The result is a brown powder mixture of complexes containing phosphoric
    0 acid 6 and water 5%. Product properties are similar to those shown in example 1.
    权利要求:
    Claims (1)
    [1]
    METHOD FOR PRODUCING INCLUSION COMPLEXES OF CYCLODEXTRINS by treating them with a strong inorganic acid, characterized in that, in order to obtain a stable product during storage, Y = ft- or §-cyclodextrin or their mixture with linear dextrin with a mixture ratio of 7 is used: 50: 5: 38 and the treatment is carried out with a 30-85% solution of phosphoric acid, 30-75% solution of sulfuric acid or 20-65% solution of nitric acid, in an amount of 0.25-1 ml of an acid solution 1 g of cyclodextrin at (-5) -25 C.
    1269738 A
    CM
    1269738 '
    类似技术:
    公开号 | 公开日 | 专利标题
    SU1269738A3|1986-11-07|Method for producing complexes of cyclodextrin inclusion
    US3416884A|1968-12-17|Crystalline zirconium phosphates
    KR910010128B1|1991-12-17|Colloidal dispersions of cerium | compounds and process for preparing the same
    JPH0781932A|1995-03-28|Production of ceric oxide
    EP0261560A2|1988-03-30|Titania sol and process for producing same
    JP3028375B2|2000-04-04|Apatite whisker and method for producing the same
    US2541733A|1951-02-13|Production of alkali metal carbonate perhydrates
    Chanaud et al.1994|Study of lanthanum-based colloidal sols formation
    EP1919959B1|2016-10-26|A method for preparing polyanhydroglucuronic acid and/or salts thereof
    JP2782744B2|1998-08-06|Method for producing binderless zeolite molded body
    Gunawardane et al.1987|Studies on Clathrasils. X. The effect of “help gases” on the formation and stability of clathrasils
    JPH07103154B2|1995-11-08|Method for producing stable α-L-aspartyl-L-phenylalanine methyl ester
    EP0451958B1|1994-12-07|Method for preparing zircon powder
    EP1105345B1|2003-10-08|Method for producing mononatrium trihydrogen pyrophosphate
    EP0511489A1|1992-11-04|Process for the synthesis of siliconnitride with a small crystal size
    US2901318A|1959-08-25|Potassium monopersulfate hydrate and its production
    US5932107A|1999-08-03|Method of separating at least one metal present in a solution by fixation onto a chitosane
    SU1701627A1|1991-12-30|Method of producing stabilized powdered red phosphorus
    US4421728A|1983-12-20|Stabilization of red phosphorus
    US5250480A|1993-10-05|Method for preparing zircon powder
    JP3022607B2|2000-03-21|Production of free-flowing hydrated ferrous sulfate.
    SU1407929A1|1988-07-07|Method of modifying cellullose nitrates
    US3513006A|1970-05-19|Process for the preparation of a mixed pigment
    KR100192711B1|1999-06-15|Production method of inorganic microbicide with silver
    CA1178788A|1984-12-04|Stabilization of red phosphorus
    同族专利:
    公开号 | 公开日
    BE890759A|1982-02-15|
    DE3141165A1|1982-06-03|
    YU42731B|1988-12-31|
    CS221994B2|1983-04-29|
    FI67224B|1984-10-31|
    FR2492359B1|1985-01-04|
    FR2492359A1|1982-04-23|
    NO154308B|1986-05-20|
    IT8168330D0|1981-10-15|
    GB2086405A|1982-05-12|
    HU182217B|1983-12-28|
    FI813213L|1982-04-18|
    NO813507L|1982-04-19|
    US4365061A|1982-12-21|
    CH649091A5|1985-04-30|
    NL8104714A|1982-05-17|
    IT1146710B|1986-11-19|
    GB2086405B|1984-01-11|
    SE448465B|1987-02-23|
    SE8106143L|1982-04-18|
    YU246581A|1983-06-30|
    NO154308C|1986-09-03|
    AT377769B|1985-04-25|
    ATA439981A|1984-09-15|
    FI67224C|1985-02-11|
    JPS57129809A|1982-08-12|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    US4054736A|1970-06-10|1977-10-18|Ono Pharmaceutical Co., Ltd.|Clathrate compounds of prostaglandins or their analogues with cyclodextrin|
    JPS5738569B2|1974-03-27|1982-08-16|
    HU176215B|1978-01-27|1981-01-28|Chinoin Gyogyszer Es Vegyeszet|Process for preparing a cyclodextrin-indomethacin inclusion complex with a ratio of at about 2:1|
    HU177419B|1978-07-13|1981-10-28|Chinoin Gyogyszer Es Vegyeszet|Process for preparing threedimensional,retentive polymers consisting of cyclodextrin and polyvinylalcohol units,capable of forming inclusion complexes in the form of bead,fibre or mainly block|
    JPS5522616A|1978-08-04|1980-02-18|Tokyo Tanabe Co Ltd|Bile acid inclusion compound and injection containing the same|
    JPS588714B2|1979-04-05|1983-02-17|Kyoshin Kk|JPS6245226B2|1983-10-11|1987-09-25|Fujisawa Pharmaceutical Co|
    IT1196033B|1984-02-22|1988-11-10|Chiesi Farma Spa|COMPOUND WITH ANTI-INFLAMMATORY ACTIVITY OBTAINED BY COMPLEXATION WITH BETA-CYCLODEXTRINE AND RELATED PHARMACEUTICAL FORMULATIONS|
    JPS6326766B2|1984-03-27|1988-05-31|Nippon Ekisho Kk|
    US4539399A|1984-07-27|1985-09-03|Advanced Separation Technologies Inc.|Bonded phase material for chromatographic separations|
    US4897472A|1986-11-19|1990-01-30|Oy Alko Ab|Process for isolation and purification of cyclodextrins|
    CA2013485C|1990-03-06|1997-04-22|John Michael Gardlik|Solid consumer product compositions containing small particle cyclodextrin complexes|
    US5139687A|1990-05-09|1992-08-18|The Proctor & Gamble Company|Non-destructive carriers for cyclodextrin complexes|
    US5384186A|1990-05-09|1995-01-24|The Proctor & Gamble Company|Non-destructive carriers for cyclodextrin complexes|
    US5246611A|1990-05-09|1993-09-21|The Procter & Gamble Company|Non-destructive carriers for cyclodextrin complexes|
    JP2976154B2|1991-11-27|1999-11-10|コニカ株式会社|Solid processing agents for silver halide photographic materials|
    IT1263831B|1993-01-29|1996-09-04|Paolo Chiesi|MULTI-COMPONENT INCLUSION COMPLEXES WITH HIGH SOLUBILITY CONSTITUTED BY A BASIC-TYPE DRUG, AN ACID AND A CYCLODEXTRINE|
    US5505866A|1994-10-07|1996-04-09|The Procter & Gamble Company|Solid particulate fabric softener composition containing biodegradable cationic ester fabric softener active and acidic pH modifier|
    US5460736A|1994-10-07|1995-10-24|The Procter & Gamble Company|Fabric softening composition containing chlorine scavengers|
    US6287603B1|1999-09-16|2001-09-11|Nestec S.A.|Cyclodextrin flavor delivery systems|
    KR20080023682A|2005-06-13|2008-03-14|카아길, 인코포레이팃드|Cyclodextrin inclusion complexes and methods of preparing same|
    MX2007015871A|2005-06-13|2008-03-04|Cargill Inc|Cyclodextrin inclusion complexes and methods of preparing same.|
    JP2009539978A|2006-06-13|2009-11-19|カーギルインコーポレイテッド|Large particle cyclodextrin inclusion complex and method for producing the same|
    MX2009007084A|2006-12-27|2009-08-20|Cargill Inc|Cyclodextrin inclusion complexes and methods of preparing same.|
    US20080283693A1|2007-05-15|2008-11-20|Evans Michael J F|Propulsion apparatus and system|
    IT1398580B1|2010-03-08|2013-03-01|Torino Politecnico|CYCLODESTRINIC NANOSPUGNE BY APPLICATION IN THE FIELD OF DELAY TO THE FLAME OF POLYMERIC MATERIALS|
    CA2849025C|2011-09-23|2017-01-17|Emerald Hilton Davis, Llc|Self-assembled nano-structured particle and method for preparing|
    US10988618B2|2011-09-23|2021-04-27|Dystar Hilton Davis Corp.|Self-assembled nano-structured particle and methods for preparing|
    GB2592599A|2020-03-03|2021-09-08|Devlin Seamus|Expansion joint cover|
    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    HU802522A|HU182217B|1980-10-17|1980-10-17|Process for producing inclusive complexes of cyclodextrines and strong inorganic oxyacids|
    [返回顶部]