- Preparation method of high-purity cis-2,6-dimethylmorpholine
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The invention relates to the technical field of chemical synthesis of medicines, and discloses a preparation method of high-purity cis-2,6-dimethylmorpholine. The method comprises the following steps:subjecting a cis-2,6-dimethylmorpholine-rich mixture of cis-2,6-dimethylmorpholine, trans-2, 6-dimethylmorpholine, cis-2,5-dimethylmorpholine and trans-2,5-dimethylmorpholine to salt formation with micromolecular aliphatic carboxylic acid in an ester solvent, and carrying out recrystallizing to obtain cis-2,6-dimethylmorpholine carboxylate; and dissociating the cis-2,6-dimethylmorpholine carboxylate by using a strong alkaline substance to obtain the high-purity cis-2,6-dimethylmorpholine. According to the method disclosed by the invention, environment-friendly ethyl acetate, isopropyl acetateand butyl acetate are used as reaction solvents and also used as recrystallization solvents, so realization of green production is facilitated which reduction of pollution is realized, impurity content is effectively controlled, finished product purity reaches 99.9% or above, used acids and solvents are friendly to environment, and the method is suitable for industrial production.
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Paragraph 0032-0034
(2020/08/22)
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- Purification method of cis-2, 6-dimethylmorpholine
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The invention discloses a purification method of cis-2, 6-dimethylmorpholine, and the method comprises the following steps: providing a mixture of cis-2, 6-dimethylmorpholine, trans-2, 6-dimethylmorpholine, cis-2, 5-dimethylmorpholine and trans-2, 5-dimethylmorpholine, reacting the mixture with carboxylic acid in an ester solvent, and crystallizing to obtain cis-2, 6-dimethylmorpholine carboxylate, wherein the content of the cis-2, 6-dimethylmorpholine in the mixture is greater than or equal to 80 mol%, and hydrolyzing the cis-2, 6-dimethylmorpholine carboxylate with an alkaline substance to obtain the cis-2, 6-dimethylmorpholine. According to the method, the raw material is easy to obtain, the raw material selection range is wider, the process is simple and convenient, the cost is low, the used reagent is environmentally friendly, the purity of the finished product is high, and the use requirements of medicine and other fields can be met.
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Paragraph 0054-0055
(2020/04/17)
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- A concise and efficient synthesis of substituted morpholines
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A simple and efficient method has been developed for the synthesis of substituted morpholines by a sequence of coupling, cyclization, and reduction reactions of easily available amino alcohols and α-halo acid chlorides. Various mono-, di-, and trisubstituted morpholines, spiro morpholines, and ring-fused morpholines, as well as morpholine homologues, were synthesized in good to excellent yields by a single methodology under similar reaction conditions. The method was also used in a multigram synthesis of (3S)-3-methylmorpholine.
- Dugar, Sundeep,Sharma, Amit,Kuila, Bilash,Mahajan, Dinesh,Dwivedi, Sandeep,Tripathi, Vinayak
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- 2,3,4,5-TETRAHYDRO-1H-1,5-BENZODIAZEPINE DERIVATIVE AND MEDICINAL COMPOSITION
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The present invention has its object to provide a 2,3,4,5-tetrahydro-1H-1,5-benzodiazepine derivative represented with the Formula (1) , or the pharmaceutically acceptable salt, which is effective as a therapeutic and prophylactic agent for diabetes, diabetic nephropathy, or glomerulosclerosis.
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