Method for separating and enriching organic matter molecules containing trans-cyclohexyl

Abstract

The invention discloses a method for separating and enriching trans-cyclohexyl-containing organic molecules, which comprises the following steps: 1, dissolving a raw material mixture to be separated in a first solvent to obtain a solution A; 2, dissolving thiourea in formamide to obtain a solution B; 3, adding the solution B into the solution A while stirring; 4, cooling to 0-5 DEG C, adding a second solvent when granular crystals are found, and continuing to carry out heat preservation and stirring; cooling to -30 to -0 DEG C until all mixed amides are fully crystallized and separated out, and filtering to obtain a mixture crystal; 5, adding a first solvent into the mixture crystal, heating and stirring to completely melt and dissolve the crystal; stopping stirring, sampling and analyzingthe content of organic matter molecules of the trans-cyclohexyl, and repeating the step 4-5 until the requirement is met when the content does not meet the requirement. The process provided by the invention is simple to operate, simplifies the operation of recovering important auxiliary materials such as thiourea, and improves the recovery rate; the quantity of three wastes and the total cost areobviously reduced.

Description

technical field [0001] The invention belongs to the field of separation and purification, and in particular relates to a separation and enrichment method for organic molecules containing trans-cyclohexyl. Background technique [0002] In the preparation and purification of organic substances in the fields of liquid crystal materials, medicine, pesticides, etc., it is often necessary to separate or enrich organic substances containing only trans-cyclohexyl from a mixture of isomers containing both cis and trans-cyclohexyl . The molecular structural formula of organic matter containing two isomers of cis and trans cyclohexyl is as follows: [0003] [0004] R1 and R2 in the above molecular structure formula are various substituents common in organic molecules other than hydrogen atoms, such as aliphatic groups, aromatic groups, halogens, ester groups, amino groups, nitro groups, cyano groups, or combinations thereof Group, etc. (the same below). [0005] At present, ther...

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Problems solved by technology

[0010] The shortcoming of above-mentioned clathrate crystallization method is: at first, need to carry out two purification separations: the first separation of crystalline clathrate and crystallization mother liquor, the second separation target product (organic matter containing trans-cyclohexyl) and thiourea (or Cyclodextrin)

[0013] The shortcoming of above-mentioned configuration conversion method is: at first, the chemical reaction that makes the generation configuration conversion of cyclohexyl is a reversible reaction, the conversion rate for some organic molecules is not high, even only about 50%

Secondly, most of this type of chemical reaction is a carbocation rearrangement mechanism. While the configuration is transformed, some isomer impurities that are difficult to remove are often produced due to the carbocation rearrangement, such as cyclohexyl rearrangement. Impurities that become five-membered rings, etc.

Again, most of the catalysts for this type of chemical reaction use Lewis acid. If the organic molecule contains ethylenic bond, ether bond, hydroxyl group, carbonyl group, amino group, etc., it is easy to have side reactions under the action of Lewis acid, or reduce the activity of Lewis acid. group, the type of organic compound cannot use the configuration transformation method

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