Production process of N-benzyl hydroxylamine hydrochloride
A benzylhydroxylamine hydrochloride and a production process technology are applied in the production process field of N-benzylhydroxylamine hydrochloride, which can solve the problems of low yield and low cost of N-benzylhydroxylamine hydrochloride, and achieve catalytic Good effect, slow volatilization rate, mild reaction effect
Inactive Publication Date: 2022-04-08
苏州诚和医药化学有限公司
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Problems solved by technology
[0003] The commonly used synthesis method of N-benzylhydroxylamine hydrochloride is to directly utilize the benzylation reaction of hydroxylamine to carry out synthesis. The cost
Method used
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preparation example 1
[0038] Add hydroxylamine hydrochloride into methanol, and the weight ratio of hydroxylamine hydrochloride to methanol is 1:7, and stir evenly to obtain ammonia solution.
preparation example 2
[0040] The difference between Preparation Example 2 and Preparation Example 1 is that the weight ratio of hydroxylamine hydrochloride to methanol is 1:8.
preparation example 3
[0042] The difference between Preparation Example 3 and Preparation Example 1 is that the weight ratio of hydroxylamine hydrochloride to methanol is 1:9.
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The invention relates to an organic synthesis intermediate, and particularly discloses a production process of N-benzyl hydroxylamine hydrochloride, which comprises the following steps: oxidation: dissolving dibenzylamine in a solvent, and adding an oxidizing agent for oxidation reaction under the catalysis of a metal oxide to obtain an oxide; ammonolysis: dissolving the oxide in an ether solvent, adding an ammonolysis solution, and carrying out ammonolysis to obtain N-benzyl hydroxylamine hydrochloride; the ammonolysis solution is a mixture of methanol and hydroxylamine hydrochloride. According to the preparation method of the N-benzyl hydroxylamine hydrochloride, few byproducts are obtained, the metal oxide is used as the catalyst, the catalytic effect is good, the oxidation reaction efficiency and the oxidation reaction conversion rate are improved, the oxide is dissolved in the ether solvent, the ammonolysis reaction conversion rate is improved, and the yield of the N-benzyl hydroxylamine hydrochloride is improved. Therefore, the yield of the N-benzyl hydroxylamine hydrochloride is improved.
Description
technical field [0001] The application relates to an organic synthesis intermediate, in particular to a production process of N-benzyl hydroxylamine hydrochloride. Background technique [0002] As an important intermediate in organic synthesis, N-benzylhydroxylamine hydrochloride plays an important role in nitrone chemistry. N-benzylhydroxylamine hydrochloride is condensed with aldehydes and ketones or added to C-C triple bonds to generate N-benzyl nitrone, and the resulting nitrone undergoes 1,3-cycloaddition reaction, which is a kind of isoxazole effective method of morphine. This method is often used to synthesize biologically active compounds and plays a unique role in drug synthesis. [0003] The commonly used synthesis method of N-benzylhydroxylamine hydrochloride is to directly utilize the benzylation reaction of hydroxylamine to carry out synthesis. The cost of this synthesis method is relatively low, but the main product of the reaction is N,N-dibenzylhydroxylamin...
Claims
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Login to view more IPC IPC(8): C07C239/10C07C291/04F26B11/18F26B25/04
Inventor 陈晓强夏秋景方欢王利民
Owner 苏州诚和医药化学有限公司
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