Salt of 3-amino-tetrahydropyrane derivative, polycrystalline type, preparation method and application thereof
A technology of crystal form and pyran, applied in the field of salts of 3-aminotetrahydropyran derivatives and their polymorphs, their preparation and application, can solve the problem of lack of long-acting drugs, lack of DPP-2/8/ 9 Enzyme selectivity, inhibitory activity is not satisfactory, etc.
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
preparation example Construction
[0140] In the preparation of the above-mentioned acid addition salt, there are no special restrictions on the solvent used and its ratio, as long as it does not hinder the reaction and has a certain solubility to the raw materials, for example: alcohols with 1-10 carbon atoms , hydrocarbons (including alkanes, halogenated alkanes, alkenes, alkynes and aromatics), ethers (including chain ethers and cyclic ethers (such as furans (including tetrahydrofuran) and dioxane class)), ketones, nitriles or esters, such as methanol, ethanol, isopropanol, chloroform (chloroform), tetrahydrofuran, acetone, methyl tert-butyl ether, ethyl acetate or acetonitrile, or by A mixed solvent formed by two or more solvents, the mixed solvent refers to a mixed solvent composed of two or more organic solvents in a certain volume ratio, or a mixed solvent composed of an organic solvent and water in a certain volume ratio . The ratio of the above-mentioned organic solvent can be any feasible ratio, incl...
preparation example 1
[0159] Preparation Example 1: Formula (I) compound (2R,3S,5R)-2-(2,5-difluorophenyl)-5-(5-(methylsulfonyl)isoindole The preparation method of hydrin-2-yl)tetrahydro-2H-pyran-3-amine
[0160]
[0161] The first step: (2R,3S,5R)-2-(2,5-difluorophenyl)-5-(5-(methylsulfonyl)isoindoline-2-yl)tetrahydro-2H-pyridine Preparation of tert-butyl pyran-3-carbamate
[0162] At room temperature, 5-(methylsulfonyl)isoindoline trifluoroacetate (100 mg) and (2R,3S)-2-(2,5-difluorophenyl)-5-carbonyl-2H - tert-butylpyran-3-carbamate (199 mg, 0.6 mmL) was dissolved in MeOH (3 mL). After stirring for 4 hours, sodium cyanoborohydride (93 mg, 1.5 mmL) was added and stirred for 13 hours, a solid precipitated, the solid was filtered, and the filter cake was washed with methanol (5 mL*2) and ethyl acetate (5 mL*2), respectively. After drying, the target product (2R,3S,5R)-2-(2,5-difluorophenyl)-5-(5-(methylsulfonyl)isoindoline-2-yl)tetrahydro-2H- tert-butyl pyran-3-carbamate (29 mg), yield 17...
Embodiment 1
[0174] Embodiment 1: the preparation of free base crystal
[0175] The formula (I) compound (2R,3S,5R)-2-(2,5-difluorophenyl)-5-(5-(methylsulfonyl)isoindoline-2 obtained in the above Preparation Example 1 -yl)tetrahydro-2H-pyran-3-amine was prepared according to the following method to obtain the free base crystal form I.
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More 


