Method for preparing (Z)-N-hydroxyphenylamidine by ammonolysis method

A technology of hydroxybenzamidine and solution method, which is applied in the field of preparation of -N-hydroxybenzamidine by ammonolysis method, can solve the problems of difficult separation, low yield, difficult separation, etc., and achieve the effect of improving the conversion rate
CN112174853AActive Publication Date: 2021-01-05HUNAN JINGSHI NEW MATERIAL CO LTD
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Patent Information

Authority / Receiving Office
CN · China
Current Assignee / Owner
HUNAN JINGSHI NEW MATERIAL CO LTD
Publication Date
2021-01-05

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Abstract

The invention discloses a method for preparing(Z)-N-hydroxyphenylamidine by ammonolysis, which comprises the following steps: 1, completely or partially dissolving alpha-halogenated benzaldoxime compounds simultaneously containing E and Z two configurations by using a first solvent to obtain a solution A; 2, adding an anhydrous sodium salt or potassium salt of a benzohydroxamic acid compound, andstirring to fully convert the (E)-alpha-halogenated benzaldoxime compound into (Z) type to obtain a solution B; 3, adding an anhydrous ammonia source, and carrying out an ammonolysis reaction to generate (Z)-N-hydroxybenzamidine so as to obtain a solution C; 4, concentrating the solution C, and adding water and a second solvent to dissolve most of solids; filtering and separating liquid; and carrying out post-treatment to obtain the high-purity (Z)-N-hydroxyphenylamidine. According to the method disclosed by the invention, the E configuration in the raw material can be fully converted into theZ configuration, the problem that more alkaline hydrolysis side reactions occur during E and Z configuration conversion reaction and ammonolysis reaction is also avoided, and the yield of the purified target product is increased to 95% or above.
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Description

technical field

[0001] The invention belongs to the field of medicine and chemical industry, and relates to a method for preparing (Z)-N-hydroxybenzamidine by ammonolysis. Background technique

[0002] N-Hydroxybenzamidine compounds are a class of intermediates widely used in medicine, pesticides, organic materials, and organic fine chemical industries; this type of compound has two isomers of E and Z configurations, and its molecular structure is The general formula is as follows:

[0003]

[0004] R in the above general formula is various common substituents on the benzene ring, such as aliphatic group, aromatic group, halogen, ester group, amino group, nitro group, cyano group, or their combination groups, etc. (hereinafter the same ).

[0005] N-hydroxybenzamidine compounds are the most commonly used and one of the cheapest preparation methods, which is to carry out ammonolysis reaction with α-halogenated benzaldoxime compounds; and this ammonolysis reaction is used...

Claims

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