- Crystal form and preparation method of clomipamine hydrochloride
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The invention belongs to the technical field of medicine crystal forms, and particularly relates to a clomipamine hydrochloride crystal form and a preparation method, and the melting point of clomipamine hydrochloride is 185.1-188.6 DEG C, in an X-ray diffraction pattern scanned by CuK alpha radiation and 2theta (degrees, +/-0.2), diffraction peaks exist at 5.70 degrees, 17.17 degrees, 19.77 degrees and 22.98 degrees, the relative abundance exceeds 50%, diffraction peaks exist at the positions of 20.21 degrees and 28.83 degrees, the relative abundance is 30%-50%, the clomipamine hydrochloridehas diffraction peaks at 23.67 degrees, 24.68 degrees and 29.99 degrees, the relative abundance is 10%-20%, the purity of the clomipamine hydrochloride is high and reaches 99.9%, the single maximum impurity content is 0.02%, and the stability is good.
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Paragraph 0027; 0034-0039
(2021/03/11)
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- High-purity clomipamine hydrochloride and preparation method thereof
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The invention relates to high-purity clomipamine hydrochloride and a preparation method thereof. Specifically, the preparation method comprises the following steps: reacting bromochloropropane with dimethylamine in the presence of alkali to obtain an intermediate I compound; adding 3-chlor-5-acetyl diphenyl imide and potassium hydroxide into toluene, and heating for reaction to obtain an intermediate II; adding potassium carbonate, potassium hydroxide into the intermediate II, and heating reactants, then adding a mixed solution of the intermediate I compound and methylbenzene, continuously heating to finish the reaction, then cooling the reaction solution, and adding water for extraction to obtain an organic layer containing clomipamine; concentrating the previous product under reduced pressure to obtain an oily substance, adding acetone, dropwise adding hydrochloric acid for acidification, crystallizing, centrifuging to obtain a crystal, and drying to obtain a clomipamine hydrochloride crude product; and adding the obtained clomipamine hydrochloride crude product and a solvent into a reaction kettle, heating for dissolving, adding medicinal carbon for reflux decolorization treatment, filtering for decarburization, cooling for crystallization, filtering for crystallization, and drying to obtain a clomipamine hydrochloride finished product. The method has the effects described in the specification.
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Paragraph 0084-0086; 0089; 0097-0106; 0112-0118; 0124-0129
(2020/11/23)
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- Efficient synthesis of tertiary amine by direct N-alkylation of secondary amine with carboxylic acid using Ni (0) encat catalyst
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In this article, direct N-alkylation of secondary amines with carboxylic acid is described. Readily available diversified carboxylic acid has been explored on variant secondary amines using encapsulated Nickel as catalyst and inexpensive sodium borohydrid
- Quadri, Syed Aziz Imam,Das, Tonmoy C.,Jadhav, Shivaji,Farooqui, Mazahar
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supporting information
p. 267 - 277
(2018/01/08)
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