Preparation method of oxalyl coenzyme A

文档序号:1137775 发布日期:2020-10-09 浏览:12次 中文

阅读说明:本技术 草酰基辅酶a的制备方法 (Preparation method of oxalyl coenzyme A ) 是由 范伟 杨建立 李鹏飞 王占旗 何琦瑜 郑绍建 于 2020-06-28 设计创作,主要内容包括:本发明公开了一种草酰基辅酶A的制备方法,具体包括以下步骤:S1,配制对甲基苯硫酚乙醚溶液;S2,量取草酰氯溶液;S3,将对甲基苯硫酚乙醚溶液添加到草酰氯中反应;S4,在反应产物中加入超纯水、静置分层;S5,移取上层溶液旋转蒸干获得草酰基对甲基苯硫酯;S6,配制草酰基对甲基苯硫酯的饱和溶液;S7,配制辅酶A溶液;S8,草酰基对甲基苯硫酯饱和溶液和辅酶A溶液反应;S9,在反应体系中加入无水乙醚分离反应产物;S10,干燥草酰基辅酶A水溶液获得草酰基辅酶A固体粉末;本发明制备过程简单,有毒有害物质使用量减少,操作人员与毒性物质接触时间缩短,反应产物的产率提高。(The invention discloses a preparation method of oxalyl coenzyme A, which specifically comprises the following steps: s1, preparing a p-methyl thiophenol ether solution; s2, measuring oxalyl chloride solution; s3, adding p-methylthiophenol ethyl ether solution into oxalyl chloride for reaction; s4, adding ultrapure water into the reaction product, standing and layering; s5, removing the upper layer solution, and performing rotary evaporation to obtain oxalyl p-methyl benzene thioester; s6, preparing a saturated solution of oxalyl p-methyl benzene thioester; s7, preparing a coenzyme A solution; s8, reacting oxalyl p-methylthiophenyl ester saturated solution with coenzyme A solution; s9, adding anhydrous ether into the reaction system to separate the reaction product; s10, drying the oxalyl-CoA water solution to obtain solid oxalyl-CoA powder; the preparation method has the advantages of simple preparation process, reduced usage amount of toxic and harmful substances, shortened contact time between operators and the toxic substances, and improved yield of reaction products.)

1. The preparation method of oxalyl coenzyme A is characterized by comprising the following steps:

s1, preparing p-methylthiophenol ethyl ether solution with the molar concentration of 1mol/L by using anhydrous ethyl ether;

s2, removing oxalyl chloride and placing the oxalyl chloride into a centrifugal tube with the volume of 1 mL;

s3, adding the p-methyl thiophenol ether solution into oxalyl chloride to react to generate a yellow transparent solution;

s4, adding ultrapure water into the yellow transparent solution until no bubbles are generated, and standing for layering;

s5, transferring the upper turbid water layer, completely evaporating the upper turbid water layer in a rotary evaporator, and removing separated yellow organic liquid in time when evaporating the upper turbid water layer to dryness to obtain oxalyl p-methyl benzene thioester;

s6, preparing a saturated solution of oxalyl p-methylphenyl thioester by using ultrapure water, and standing for 30S at 50 ℃;

s7, preparing a coenzyme A solution with the molar concentration of 0.5mol/L by using ultrapure water;

s8, adding the coenzyme A solution into a saturated solution of oxalyl p-methyl benzene thioester, blowing uniformly, and reacting for 20 min;

s9, adding anhydrous ether into the reaction system, blowing, beating and mixing uniformly, placing the reaction system in a centrifuge with the rotating speed of 12000rpm, centrifuging for 10min, layering, and absorbing a water layer to obtain an oxalyl coenzyme A water solution;

s10, placing the oxalyl-CoA water solution in a vacuum drier and centrifuging to obtain solid oxalyl-CoA powder.

2. The method of producing oxalyl-CoA according to claim 1, wherein the volume ratio of the p-methylthiophene ether solution to oxalyl chloride in S3 is (8: 1) to (6: 1).

3. The method of preparing oxalyl-coa according to claim 1, wherein the volume ratio of saturated solution of oxalyl-p-methylbenzyl thioester to coa in S8 is 40: 1.

4. the method of claim 1, wherein the temperature of the vacuum drier in S10 is 4 ℃, the centrifugation time is 2min, and the centrifugation speed is 12000 rpm.

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