2results about How to "Avoid separation and purification" patented technology

This invention discloses a method for synthesizing potassium 4-methoxysalicylate based on supramolecular-assisted methylation, belonging to the field of organic synthesis technology. The process is based on supramolecular chemistry principles and includes the following steps: (1) Preparation of a macrocyclic host molecule-methylating agent complex loaded with a methylating agent: The macrocyclic host molecule and the methylating agent are reacted at pH 7-9 and 25-40℃ to form a complex solution; (2) One-pot preparation of the target product: 2,4-dihydroxybenzoic acid is salted with potassium hydroxide, potassium carbonate is added, and the above complex solution is added dropwise. A selective methylation reaction is carried out at 55-65℃. After the reaction is complete, post-treatment yields the product. This invention utilizes the molecular recognition function of the macrocyclic host to achieve highly selective methylation of the 4-hydroxyl group under mild conditions. This process has the advantages of simple operation, high safety, low waste, and recyclable host molecules. The yield of potassium 4-methoxysalicylate can reach over 85%, and the purity exceeds 99.0%.

The invention discloses a synthesis method of cis-4-methoxy cyclohexylamine hydrochloride, and belongs to the technical field of organic chemistry. The synthesis method comprises the following steps: 1, introducing air to react N-(benzyloxycarbonyl) hydroxylamine and 1, 3-cyclohexadiene under the catalysis of copper tetraphenylporphyrin to generate a compound I; 2, generating a compound II from the compound I and sodium methoxide under the action of boric acid ester; and 3, carrying out catalytic hydrogenation on the compound II, and reacting with hydrogen chloride to obtain the cis-4-methoxy cyclohexylamine hydrochloride. The method is simple to operate, and dangerous hydrogenation reaction conditions under high temperature and high pressure for reducing benzene rings are avoided; under the mediation of boric acid ester, the regioselectivity and stereoselectivity of the ring-opening reaction of sodium methoxide and a compound I are controlled to obtain a compound II with a cis-structure, and the compound II is subjected to catalytic hydrogenation and acidification salification to obtain a high-purity cis-stereoconfiguration product, so that a new path is provided for synthesis of cis-4-methoxy cyclohexylamine hydrochloride.