61717-82-6Relevant articles and documents
The crystal structure of the Dess-Martin periodinane
Schroeckeneder, Albert,Stichnoth, Desiree,Mayer, Peter,Trauner, Dirk
, p. 1523 - 1527,5 (2012)
We report the elusive X-ray structure of the Dess-Martin periodinane (DMP), a hypervalent iodine reagent popular amongst synthetic chemists. In the solid state, the highly crystalline compound forms an intricate coordination polymer held together by intermolecular halogen and hydrogen bonds.
Process for preparing Dess-Martin reagent through solid superacid catalysis
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Paragraph 0014; 0021-0022; 0024-0025; 0027-0028; 0030-0031, (2021/07/31)
The invention belongs to the technical field of organic synthesis, and discloses a process for preparing a Dess-Martin reagent through solid superacid catalysis. The process comprises the following steps of: S1, oxidation reaction, specifically, mixing potassium bromate and tap water, adding solid superacid HERD-Cat-1, stirring and heating the materials to 40-90 DEG C; adding o-iodobenzoic acid in batches, reacting for 1-8 hours at the temperature after addition of the o-iodobenzoic acid, performing cooling, and then centrifugally washing a product with water and washing with an organic solvent to obtain an IBX wet product; S2, acetylation reaction, specifically, adding the IBX wet product into an organic solvent, performing dissolving and filtering, recovering solid superacid HERD-Cat-1, adding a catalyst and acetic anhydride, heating to 40-80 DEG C, performing a reaction, performing cooling and crystallizing, and performing centrifugation and drying to obtain the Dess-Martin reagent. After the solid superacid is used for catalysis, generation of a large amount of waste acid is avoided, and meanwhile the purity of IBX is high. The process has the advantages of short reaction steps, high chemical purity, simplicity in operation, low cost, high production safety, environmental friendliness and the like, and is suitable for industrial production.
Preparation method of β - carotene with high total trans content
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Paragraph 0047-0049, (2021/09/01)
The invention provides a preparation method of β - carotene with a high total trans content. Starting from the vitamin A derivative, C20 phosphine salt is obtained through reaction with triphenylphosphine, and the C20 phosphine salt is subjected to condensation reaction under the action IBX high iodine compound and base to obtain β - carotene containing cis-trans, and then the β - carotene with high trans content is obtained under the action of a transition metal loading catalyst. The method avoids the use of a strong oxidizing agent in the traditional process, is environmentally friendly and can reduce the peroxidation of β - carotene, so that the reaction yield is increased, and the transition metal catalyst enables the obtained β - carotene content to be full. Trans increase.
Method for preparing 2-iodoxybenzoic acid
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Paragraph 0019-0024; 0031-0035; 0063-0066, (2019/02/13)
The invention relates to a method for preparing 2-iodoxybenzoic acid, and belongs to the technical field of synthesis of rings containing a halogen atom as a heterocyclic atom. The method comprises the following steps: adding an oxidant to 2-iodobenzoic acid used as a raw material, carrying out a reaction in an acidic solution at 50-120 DEG C for 1-6 h, and purifying the obtained reaction productto obtain the 2-iodoxybenzoic acid. The method has the advantages of small toxicity, mild technologic conditions, economical and cheap property and suitableness for industrialization when applied to the synthesis of a catalyst.