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Dexketoprofen glueosceoctylamine and preparation process thereof and medicine composition having active composition of same

A technology of dexketoprofen and octylglucamine salt, which is applied in the direction of drug combination, organic active ingredients, medical preparations containing active ingredients, etc., can solve the problems of low yield and complexity of dexketoprofen, and achieve low cost , High split rate and simple process

Inactive Publication Date: 2003-05-21
NO 1 AUXILARY HOSPITAL NO 4 MILLITARY MEDICAL UNIV P L A
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This process is more complicated, and the yield of dexketoprofen is relatively low, about 30%

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] (1) Preparation of crude crystals of dexketoprofen octylglucosamine salt: (±)-ketoprofen and N-octylglucosamine are mixed with two kinds of raw materials in a molar ratio of 1: 1, and put into a solvent containing organic solvent Add it to the container containing the mixed solvent of methanol and ethyl acetate with a volume ratio of 1:1.5, the weight ratio of the raw material mixture to the mixed solvent is 1:3.5, heat and reflux at 70°C for 30 minutes, cool to room temperature, and place Cool in a refrigerator or in a water bath at 2°C for 7 hours, filter with suction, wash with a mixed solvent of methanol and ethyl acetate at a volume ratio of 1:1.5, and dry to obtain crude crystals.

[0029] (2) Recrystallization: Heat the above crude crystals and organic solvent at 70°C to completely dissolve the crude crystals, cool to 40°C, place in the refrigerator for 10 hours, filter with suction, and mix with methanol and ethyl acetate at a volume ratio of 1:1.5 Solvent washi...

Embodiment 2

[0032] (1) Preparation of crude crystals of dexketoprofen octylglucosamine salt: (±)-ketoprofen and N-octylglucosamine are mixed with two kinds of raw materials in a molar ratio of 1:0.5, and are added to a tank containing methanol and acetic acid In a solvent with ethyl ester volume ratio of 1:1 mixed solvent, the weight ratio of the raw material mixture to the mixed solvent is 1:2, heat and reflux at 60°C for 30 minutes, cool to room temperature, and place in a refrigerator or a water bath at 0°C Cool for 6 hours, filter with suction, wash with a mixed solvent of methanol and ethyl acetate with a volume ratio of 1:1, and dry to obtain crude crystals.

[0033](2) Recrystallization: Heat the above crude crystals and organic solvent at 60°C to completely dissolve the crude crystals, cool to 35°C, place in the refrigerator for 8 hours, filter with suction, and mix with methanol and ethyl acetate at a volume ratio of 1:1 Solvent washing and drying to obtain dexketoprofen octylami...

Embodiment 3

[0036] (1) Preparation of crude crystals of dexketoprofen octylglucosamine salt: (±)-ketoprofen and N-octylglucosamine are mixed with two kinds of raw materials in a molar ratio of 1:2, and are added to a tank containing methanol and acetic acid In a solvent with ethyl ester volume ratio of 1:2, the weight ratio of raw material mixture to organic solvent is 1:5, heat and reflux at 80°C for 30 minutes, cool to room temperature, and place in a refrigerator or a water bath at 5°C Cool for 8 hours, filter with suction, wash with a mixed solvent of methanol and ethyl acetate with a volume ratio of 1:2, and dry to obtain crude crystals.

[0037] (2) Recrystallization: Heat the above crude crystals and organic solvent at 80°C to completely dissolve the crude crystals, cool to 45°C, place in the refrigerator for 12 hours, filter with suction, and mix with methanol and ethyl acetate at a volume ratio of 1:2 Solvent washing and drying to obtain dexketoprofen octylamine salt.

[0038] (...

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PUM

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Abstract

The present invention relates to a dextroketoprofen glucoseoctylamine, its preparation method and medicine composition containing said active component. Its preparation method includes: preparing dextroketoprofen glucoseoctyline salt crude crystal, recrystallization to obtain dextroketoprofen glucoseoctylamine salt and recovering process of (-)-ketoprofen and N-octyl glucosamine. Said compound possesses the actions of clearing away heat, stopping pain and resisting inflammation, its medicine composition can be used for curing rheumatic and rheumatoid arthritis, ankylosing spondylitis, gouty arthritis and various pains.

Description

technical field [0001] The invention relates to a pharmaceutical compound, in particular to a dexketoprofen octylamine salt with antipyretic, analgesic and anti-inflammatory effects, a preparation method thereof and a pharmaceutical composition containing the active ingredient. technical background [0002] Ketoprofen, whose chemical name is α-methyl-3-benzoylphenylacetic acid, belongs to 2-aryl propionic acid non-steroidal anti-inflammatory analgesics, its indications are basically the same as ibuprofen, but its efficacy Stronger than ibuprofen. Ketoprofen still has a certain central analgesic effect. Clinically, ketoprofen is mainly used to treat rheumatic or rheumatoid arthritis, osteoarthritis, ankylosing spondylitis, gouty arthritis and various pains, such as dysmenorrhea, toothache, postoperative pain, cancer pain, etc. The curative effect of ketoprofen is definite, and it has been included in page 955 of the 2000 edition of the Chinese Pharmacopoeia. Ketoprofen als...

Claims

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Application Information

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IPC IPC(8): A61K31/7008A61P19/02A61P19/06A61P19/08A61P29/00C07H3/06
Inventor 张三奇顾宜方坤泉王纪保
Owner NO 1 AUXILARY HOSPITAL NO 4 MILLITARY MEDICAL UNIV P L A
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