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Improved preparing method of cis-counterpoint substituted cyclohexyl amino nitrile maleate

A technology of base amino nitrile and maleate, applied in the field of preparation of cyclohexyl amino nitrile maleate, can solve the problems of polluting products, affecting product quality, low solubility and the like

Active Publication Date: 2019-10-01
HEBEI LANSHENG BIOTECH CO LTD +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] But, because maleic acid is solid, solubility is little in reaction solvent, and the solubility of the cis-para-position substituted cyclohexyl amino nitrile maleate of salification gained is also very low, and cis body salt will be deposited on free The phenomenon that the surface of maleic acid is wrapped around it will hinder the salt formation of the wrapped free maleic acid, and finally the unsalted maleic acid will pollute the product, affecting the quality of the product

Method used

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  • Improved preparing method of cis-counterpoint substituted cyclohexyl amino nitrile maleate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] To 602kg cis / trans ratio is the toluene solution (solution total amount is 1500kg) of p-methoxycyclohexylaminonitrile of 55:45 to add 181kg (0.4mol mole times) maleic acid, after adding, maintain temperature at 25~30°C, ultrasonic vibration for 2 hours while stirring, the ultrasonic power is 0.4 W / L, then filter the precipitated maleate, rinse with an appropriate amount of toluene, and dry to obtain white cis-p-methoxycyclohexyl Aminonitrile maleate (386kg, cis / trans ratio: 95.5:4.5).

[0026] Gained product is passed through gas-phase internal standard method, take p-xylene as internal standard substance to measure the content of cyanamide maleate under the following conditions, convert the amount of maleic acid combined with cyanamide by this content, maleic acid Feed amount minus the amount of maleic acid combined with cyanamide is the amount of free maleic acid wrapped.

[0027] Gas phase conditions: FID detector

[0028] Inlet 245°C Detector: 250°C

[0029] Prog...

Embodiment 2

[0035] The time of ultrasonic vibration while stirring was adjusted to 4 hours, and the others were the same as in Example 1 to obtain white cis-p-methoxycyclohexylaminonitrile maleate (404.5kg, cis / trans ratio: 96.8:3.2).

[0036] The same method as in Example 1 records that the free maleic acid that is wrapped accounts for 4.1% of the total amount of maleic acid charged, and the decomposition rate of the obtained cis-p-methoxycyclohexylaminonitrile maleate on the 7th day is 0.37%.

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Abstract

The invention provides an improved preparing method of cis-counterpoint substituted cyclohexyl amino nitrile maleate shown in the formula (I). The method includes the steps of adding 0.3-0.55 molar fold of maleic acid to an organic solvent solution of a cis / trans-counterpoint substituted cyclohexyl amino nitrile compound corresponding to the formula (I) for stirring and ultrasonic treatment, and conducting filtering to obtain the cis-counterpoint substituted cyclohexyl amino nitrile maleate shown in the formula (I). In the formula (I), R1 represents a C1-C10 alkyl group or alkyl oxygroup, a C1-C10 vinyl group or vinyl oxygroup, a C1-C10 alkynyl group or alkynyl oxygroup, a C1-C10 naphthenic group or naphthenic oxygroup and a C1-C10 heterocyclic alkyl group or heterocyclic alkyl oxygroup with one or two heteroatoms selected from O and N, and HX represents maleic acid.

Description

technical field [0001] The invention relates to an improved preparation method of cis-para-substituted cyclohexylaminonitrile maleate. Background technique [0002] Maleic acid can separate para-substituted cyclohexylaminonitrile compounds with good selectivity, and the cis-isomer salt compound obtained after the salt separation is an important intermediate for the preparation of spirotetramat. [0003] But, because maleic acid is solid, solubility is little in reaction solvent, and the solubility of the cis-para-position substituted cyclohexyl amino nitrile maleate of salification gained is also very low, and cis body salt will be deposited on free The surface of maleic acid and its encapsulation will hinder the encapsulation of free maleic acid from forming a salt, and finally the unsalted maleic acid will pollute the product, affecting the quality of the product. Contents of the invention [0004] The inventors of the present application have found that during the prep...

Claims

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Application Information

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IPC IPC(8): C07C253/34C07C253/30C07C255/46C07C51/41C07C57/145
CPCC07C253/34C07C253/30C07C51/412C07B2200/07C07C2601/14C07C255/46C07C57/145
Inventor 郭庆春董志鹏苑立刚刘海龙郭红永
Owner HEBEI LANSHENG BIOTECH CO LTD
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