A kind of preparation method of (e)-oct-4-ene-1,8-dioic acid
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A diacid, butene technology, applied in the preparation of carboxylic acid nitrile, the preparation of organic compounds, the preparation of nitrile, etc., to achieve the effects of low input cost, high product purity, and easy control
Active Publication Date: 2021-03-23
武汉嘉诺康医药技术有限公司
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Pan Li, et al.. et al. (J.Org.Chem.1999,64,2259-2263) replaced the base with industrially available lithium diisopropylamide (LDA ), but the reaction still requires low temperature, and LDA is also flammable and explosive
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Embodiment 1
[0046] Embodiment 1: The preparation method of (E)-oct-4-ene-1,8-dioic acid comprises the following steps:
[0047] step one:
[0048]In a 500ml three-neck reaction flask equipped with a thermometer and a constant pressure dropping funnel, add tetrahydrofuran (THF) (150mL) and Mg powder 11.5g, then raise the temperature of the reaction solution to 40°C, and slowly add 5mL, 2M bromoacetonitrile dropwise therein The reaction was initiated by the THF solution, and then the temperature of the reaction solution was lowered to 10°C, and 70 mL of 2M bromoacetonitrile solution in THF was slowly added dropwise, maintaining the temperature at 10°C, and stirring was continued at 10°C for 1 hour after the addition was completed.
[0049] Then 1,4-dibromo-2-butene (0.047mol) was dissolved in THF (100ml) to prepare a solution of 1,4-dibromo-2-butene, and the prepared A good solution of 1,4-dibromo-2-butene was added dropwise to the above reaction system, and the temperature was kept at 10-...
Embodiment 2
[0052] Embodiment 2: the preparation method of (E)-oct-4-ene-1,8-dioic acid comprises the following steps:
[0053] step one:
[0054] In a 500ml three-necked reaction flask equipped with a thermometer and a constant pressure dropping funnel, add tetrahydrofuran (150ml) and 15g of zinc powder, then raise the temperature of the reaction solution to 40°C, slowly add 5mL, 2M tetrahydrofuran solution of bromoacetonitrile dropwise to initiate the reaction , and then the temperature of the reaction solution was lowered to -10°C, and 50 mL of 2M bromoacetonitrile tetrahydrofuran solution was continued to be slowly added dropwise, the temperature was maintained at 0°C during the dropwise addition, and stirring was continued at 0°C for 1 hour after the dropwise addition was completed.
[0055] Then 1,4-dibromo-2-butene (0.047mol) was dissolved in THF (100ml) to prepare a 1,4-dibromo-2-butene solution, and the prepared Add the 1,4-dibromo-2-butene solution dropwise to the above reactio...
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Abstract
The invention belongs to the chemical synthesis field, and specifically relates to a preparation method of (E)-oct-4-ene-1,8-diacid. The preparation method comprises the following steps: taking bromoacetonitrile as a starting raw material, reacting with a metal element to obtain a metal composite of bromoacetonitrile, and preparing (E)-oct-4-ene-1,8-dinitrile from the metal composite and 1,4-dibromo-2-butene; and hydrolysing (E)-oct-4-ene-1,8-dinitrile to obtain (E)-oct-4-ene-1,8-diacid. According to the method disclosed by the invention, the starting material is cheap and easily available, and a product with purity of 99% or higher can be obtained by simple post-treatment steps such as liquid-separation extraction and concentration after first-step reaction, and simple extraction after hydrolysing cyano alkali into carboxylic acid or hydrolysing cyan acid into ester in the second step. The process reaction and post-treatment operation are simple, and the obtained product is high in quality, so that using requirements can be met without further purification. The preparation method adopts an environment-friendly process, is economical and practical, and is very suitable for industrial production.
Description
technical field [0001] The invention belongs to the field of chemical synthesis, and in particular relates to a preparation method of (E)-oct-4-ene-1,8-dioic acid. Background technique [0002] (E)-oct-4-ene-1,8-dioic acid is the key intermediate of mivacurium chloride, and its structural formula is as follows: [0003] [0004] Mivacurium chloride is a non-depolarizing muscle relaxant with the following structure, and its chemical structure belongs to benzylisoquinoline compounds: [0005] [0006] Mivacurium chloride is used for endotracheal intubation and maintenance of muscle relaxation. After intravenous injection, the muscle relaxation has a rapid onset (2 minutes) and a short duration (15 minutes). . [0007] The preparation method of mivacurium chloride has many reports in the prior art, for example, European patent EP0181055A1 reports 6,7-dimethoxyl-2-methyl-1-(3,4,5-trimethoxyphenyl )-1,2,3,4-Tetrahydroisoquinoline undergoes three steps of resolution, quat...
Claims
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