Synthesis process of ketorolac

A synthesis process, a technology for ketorolac, applied in the direction of organic chemistry, etc., can solve the problems of difficult process wastewater treatment, unfavorable environmental protection, dark product color, etc., and achieves easy control of process conditions, increased process production safety, and easy operation. Effect

Inactive Publication Date: 2018-06-22
上海仁实医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] In the above documents, the synthesis of the key dicarboxylic acid intermediates requires the use of excess potassium permanganate and manganese acetate. After using manganese-containing metal salts, the process wastewater generated is difficult to treat, and the product is dark in color. Activated carbon or silica gel is required for post-treatment. Multi-step decolorization and purification, resulting in solid waste such as waste activated carbon and waste silica gel
A large amount of liquid and solid waste is not conducive to the concept of environmental protection and green economic chemistry, therefore, a new solution needs to be proposed to solve the above technical problems

Method used

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  • Synthesis process of ketorolac
  • Synthesis process of ketorolac
  • Synthesis process of ketorolac

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Embodiment 1

[0036] Embodiment 1: a kind of synthetic technique of ketorolac, press figure 1 The reaction formula in carries out, and it comprises the following steps:

[0037] Step 1, the synthesis of compound 3: add 5 equivalents of pyrrole, 1 equivalent of dimethyl iodomalonate to the reaction flask, then add dimethyl sulfoxide and 0.1 equivalent of iron salt catalyst, the iron salt catalyst is ferrous sulfate heptahydrate, The weight ratio of dimethyl sulfoxide to dimethyl iodomalonate is 2:1. Add 5 equivalents of oxidant dropwise to the flask under stirring at room temperature. The oxidant is hydrogen peroxide. The dropwise addition time is 0.5 hours. After the dropwise addition is complete, continue to stir React for 0.5 hours, then add 5 equivalents of dichloroethane, separate the phases, wash the organic phase twice with 10ml of water, dry with a desiccant, the desiccant is anhydrous sodium sulfate, filter, and concentrate the filtrate until no liquid flows out. Distill the remain...

Embodiment 2

[0042] Embodiment 2: a kind of synthetic technique of ketorolac, differs from embodiment 1 in that, comprises the following steps:

[0043] Step 1, the synthesis of compound 3: add 13 equivalents of pyrrole, 1 equivalent of dimethyl iodomalonate to the reaction flask, then add dimethyl sulfoxide and 0.3 equivalents of iron salt catalyst, the iron salt catalyst is ferrous sulfate heptahydrate, The weight ratio of dimethyl sulfoxide to dimethyl iodomalonate is 3:1. Add 10 equivalents of oxidant dropwise into the flask under stirring at room temperature. The oxidant is hydrogen peroxide. The dropwise addition time is 0.8 hours. After the dropwise addition is complete, continue to stir React for 0.8 hours, then add 10 equivalents of dichloroethane, separate the phases, wash the organic phase twice with 10ml of water, dry with a desiccant, the desiccant is anhydrous sodium sulfate, filter, and concentrate the filtrate until no liquid flows out. Distill the remaining pyrrole under r...

Embodiment 3

[0047] Embodiment 3: a kind of synthetic technique of ketorolac, differs from embodiment 1 in that, comprises the following steps:

[0048] Step 1, the synthesis of compound 3: add 20 equivalents of pyrrole, 1 equivalent of dimethyl iodomalonate to the reaction flask, then add dimethyl sulfoxide and 0.5 equivalents of iron salt catalyst, the iron salt catalyst is ferrous sulfate heptahydrate, The weight ratio of dimethyl sulfoxide to dimethyl iodomalonate is 5:1. Add 15 equivalents of oxidant dropwise into the flask under stirring at room temperature. The oxidant is hydrogen peroxide. The dropwise addition time is 1 hour. After the dropwise addition is complete, continue to stir React for 1 hour, then add 15 equivalents of dichloroethane, separate the phases, wash the organic phase twice with 10ml of water, dry with a desiccant, the desiccant is anhydrous sodium sulfate, filter, and concentrate the filtrate until no liquid flows out. Distill the remaining pyrrole under reduced...

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Abstract

The invention discloses a synthesis process of ketorolac, and relates to the technical field of medicine synthesis. The synthesis process solves the technical problems that the existing process can generate a large amount of liquid and solid wastes, and the environment protection is not facilitated. Hydrogen peroxide with side products being water is used as an oxidizing agent; malysite is used asa catalyst; a large number of manganese salts are replaced; when 1kg of ketorolac is reduced, 3.5 to 6.1kg of discharged liquid and solid wastes are reduced; the green and environment-friendly effects are achieved. Benzoyl chloride is directly used as raw materials; the one-step reaction is reduced; the synthesis process is simpler; the methyl tertiary butyl ether is used for replacing the flammable and combustible diethyl ether; the process production safety is improved. The synthesis process has the advantages that the operation is easy; the process conditions can be easily controlled; thefinal product purification and aftertreatment are simple.

Description

technical field [0001] The invention relates to the technical field of medicine synthesis, more specifically, it relates to a synthesis process of ketorolac. Background technique [0002] The structural formula of ketorolac is shown in chemical formula 1. It is a non-steroidal anti-inflammatory drug with strong analgesic and moderate anti-inflammatory effects. The analgesic effect of this drug is equivalent to that of morphine, and stronger than that of aspirin and indomethacin and naproxen. Compared with opioid analgesics, its advantages are rapid onset, no addiction, and no respiratory depression. [0003] Its preparation, ketorolac tromethamine, is used for all pains, especially cancer visceral pain, and all kinds of pains that required morphine or pethidine to be effective in the past, and is also suitable for short-term elimination of trauma and postoperative pain, swelling Pain, severe pain and pain caused by various reasons. Tablet or injection may be used to relie...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D487/04
CPCC07D487/04
Inventor 李文杰宋东林长学
Owner 上海仁实医药科技有限公司
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