Voglibose semi-hydrated crystal, its preparation method and its uses in medicament formulation

A technology for voglibose and hemihydrate, which is applied in the field of preparation of voglibose hemihydrate crystals, and can solve the problems of insufficient crystal precipitation, low yield, and increased processes.

Inactive Publication Date: 2007-08-01
PHARMAXYN LAB
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method needs to consume a large amount of methanol or ethanol, and the crystallization is insufficient, so the yield is not high; the obtained crystal particle size is not uniform enough, and further pulverization is required, resulting in more processes and higher production costs.

Method used

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  • Voglibose semi-hydrated crystal, its preparation method and its uses in medicament formulation
  • Voglibose semi-hydrated crystal, its preparation method and its uses in medicament formulation
  • Voglibose semi-hydrated crystal, its preparation method and its uses in medicament formulation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0086] Example 1 (1S)-(1(hydroxy), 2,4,5 / 1,3)-5-[(2-hydroxy-1-(hydroxymethyl)ethyl)amino]-1-carbon-hydroxy Preparation of methyl-1,2,3,4-cyclohexanetetraol hemihydrate crystals (voglibose hemihydrate crystals)

[0087] Dissolve tetrabenzyl voglibose (300.0g, 0.48mol) in 90% formic acid / methanol (1:19, 6L), add palladium black (60g), react at room temperature for 12 hours under nitrogen protection, and filter Wash with methanol / water (1:1) 2L, concentrate the filtrate, absorb the residue with strong acid ion exchange resin (5L), wash with water, and then eluted with 0.5N ammonia water. After the eluent is evaporated to remove water, add no 2L of water and ethanol, stirring, filtering the precipitated light gray crystals, and vacuum drying for 12 hours to obtain 110 g of crude voglibose.

[0088] Dissolve 100g of the above crude voglibose in 200g of hot pure water, add 200g of ethanol, 10g of activated carbon, heat at 60°C for 30 minutes to decolor, filter, add 500g of ethanol at 60...

Embodiment 2

[0090] Example 2 Preparation of voglibose hemihydrate crystals

[0091] Dissolve 100g of the crude voglibose (the preparation method is the same as in Example 1) in 100g of hot pure water, add 100g of methanol, 10g of activated carbon, heat at 60°C for 30 minutes to decolorize, filter, add 1000g of methanol at 50°C to the filtrate, and stir. The crystals were precipitated, cooled to room temperature naturally, filtered, and dried under vacuum at 40°C for 12 hours to obtain 85 g of voglibose hemihydrate crystals.

Embodiment 3

[0092] Example 3 Preparation of voglibose hemihydrate crystals

[0093]Dissolve 100g of the crude voglibose (the preparation method is the same as in Example 1) in 300g of hot pure water, add 300g of ethanol, 10g of activated carbon, heat at 60°C for 30 minutes to decolorize, filter, and add 300g of isopropanol at 70°C to the filtrate. Crystals were precipitated under stirring, cooled to room temperature naturally, filtered, and vacuum dried at 40°C for 48 hours to obtain 90 g of voglibose hemihydrate crystals.

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Abstract

The invention discloses a Fuge train wave hemi-hydrated crystalline with 0.5 molecular crystallinic water, whose structure and character is simulated by single-crystal X-ray diffraction, powder X-ray diffraction, thermogravimetric analysis (TG), differential scanning calorimetry (DSC), infrared spectrum (IR), element analysis and specific rotation, wherein the molecular structure is C10H21NO7 .0.5H2O, which belongs to orthogonal crystal system in the P2(1)2(1)2(1) spatial group; the cell parameter a is 9.877(2); b is 9.905(2); c is 26.760(5); alpha is 90 deg; beta is 90deg; gamma is 90 deg; R is 0.0324.

Description

Technical field [0001] The invention relates to a hemihydrate crystal of voglibose, in which 0.5 molecule of water is bound to each molecule of voglibose, which has good stability. The voglibose hemihydrate crystal can lose crystal water under certain conditions and transform into another voglibose crystal without crystal water. The invention also relates to a preparation method of the voglibose hemihydrate crystal and its application in pharmaceutical preparations. Background technique [0002] Voglibose, the chemical name is (1S)-(1(hydroxy), 2,4,5 / 1,3)-5-[(2-hydroxy-1-(hydroxymethyl)ethyl)amino] -1-Carbon-hydroxymethyl-1,2,3,4-cyclohexanetetraol, which belongs to the class of α-glycosidase inhibitors for the treatment of diabetes, is a new type of diabetes treatment agent, currently available in China and South Korea And Japan marketed for the treatment of postprandial hyperglycemia. Its structural formula is shown in Figure (I) below: [0003] [0004] Oral administration o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C213/10C07C215/44A61K31/133A61P3/10
CPCC07C215/44A61P3/10
Inventor 刘立刚李瑞文
Owner PHARMAXYN LAB
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