Preparation method of oxalyl coenzyme a
An oxalyl coenzyme and oxalyl technology, which is applied in the preparation of sugar derivatives, chemical instruments and methods, sugar derivatives, etc., can solve the problems of cumbersome operation process, prone to explosion, operator injury, etc., and achieve safe reaction process, The effect of reduced consumption and complete recovery
Active Publication Date: 2021-11-12
ZHEJIANG UNIV +1
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[0002] In 1914, R. Stolle of Germany successfully synthesized oxalyl p-methylphenylthioester by using oxalyl chloride and p-methylthiophenol, which laid the foundation for the synthesis of oxalyl-CoA and provided a theoretically feasible way , but currently oxalyl-CoA has not been commercialized, and its production process has not been standardized; and the method for synthesizing oxalyl-p-methylphenylthioester proposed by R. Lively in nature, highly toxic and corrosive, p-methylthiophenol has an unpleasant odor, is flammable, explosive, highly toxic, and has a strong carcinogenic ability. During the synthesis process, the operator has a long contact time with harmful substances. It is easy to cause damage to the operator, and the preparation process includes distillation operation, which is prone to explosion, and the distillate cannot be completely condensed and refluxed, which will cause certain toxicity to the environment and operators
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[0026] 1. Reference figure 1 , the preparation method of oxalyl-CoA comprises the following steps:
[0027] S1, dissolving p-methylthiophenol in anhydrous ether solution to prepare a p-methylthiophenol ether solution with a molar concentration of 1mol / L to 2mol / L, adding p-methylthiophenol to the oxalyl chloride solution Diethyl ether solution, the volume ratio of p-methylthiophenol ether solution to oxalyl chloride solution is 4:1~3:1, oxalyl chloride as a strong electrophile reacts completely with p-methylthiophenol as a strong nucleophile, Generate transparent yellow solution, and reaction principle is as shown in formula (1);
[0028]
[0029] If the molar concentration of p-methylthiophenol ether solution decreases during the reaction, the amount of ether in the reaction system will increase, and the contact time of the staff and toxic and harmful substances will be prolonged while increasing the reaction cost. The increase of the molar concentration of the thiopheno...
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The invention discloses a preparation method of oxalyl-coenzyme A, specifically comprising the following steps: S1, preparing p-methylthiophenol ether solution, mixing and reacting the p-methylthiophenol ether solution and oxalyl chloride solution to form a yellow solution; S2, heating the yellow solution to a constant volume to obtain a brown-yellow solution; S3, reacting the brown-yellow solution with ultrapure water to form a precipitate; S4, dissolving the precipitate and using a centrifuge to separate layers; S5, absorbing the upper water layer and evaporating to dryness to obtain grass Acyl p-toluene thioester; S6, prepare oxalyl p-toluene thioester saturated solution and coenzyme A solution; S7, mix oxalyl p-toluene thioester saturated solution and coenzyme A solution for reaction; S8, in the reaction Add anhydrous ether and chloroform to the system, and centrifuge to separate layers; S9, dry the centrifuged water layer to obtain oxalyl-CoA solid powder; the preparation process of the present invention is simpler, the use of reactants is less, and the cost is lower , with better reaction security.
Description
technical field [0001] The invention belongs to the technical field of chemical synthesis, in particular to a preparation method of oxalyl-CoA. Background technique [0002] In 1914, R. Stolle of Germany successfully synthesized oxalyl p-methylphenylthioester by using oxalyl chloride and p-methylthiophenol, which laid the foundation for the synthesis of oxalyl-CoA and provided a theoretically feasible way , but currently oxalyl-CoA has not been commercialized, and its production process has not been standardized; and the method for synthesizing oxalyl-p-methylphenylthioester proposed by R. Lively in nature, highly toxic and corrosive, p-methylthiophenol has an unpleasant odor, is flammable, explosive, highly toxic, and has a strong carcinogenic ability. During the synthesis process, the operator has a long contact time with harmful substances. It is easy to cause damage to the operator, and the preparation process includes distillation operation, which is prone to explosion...
Claims
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IPC IPC(8): C07H19/207C07H1/00
CPCC07H1/00C07H19/207
Inventor 杨建立李鹏飞范伟何琦瑜郑绍建
Owner ZHEJIANG UNIV