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Industrial preparation method of 2, 6-di-O-methyl-beta-cyclodextrin and inspection method thereof

A technology of cyclodextrin and dimethylformamide, applied in 2 fields, can solve the problems of few indicators for controlling product quality, etc., and achieve the effects of good prevention of pertussis in children, strict performance testing, and significant social benefits

Active Publication Date: 2019-05-24
廊坊兴龙生物技术有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In addition to giving the molecular formula and molecular weight of the compound, some companies give the product's nuclear magnetic resonance spectrum, carbon element analysis table, Raman spectrum or mass spectrometry data, etc.; there are few indicators for controlling product quality

Method used

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  • Industrial preparation method of 2, 6-di-O-methyl-beta-cyclodextrin and inspection method thereof
  • Industrial preparation method of 2, 6-di-O-methyl-beta-cyclodextrin and inspection method thereof
  • Industrial preparation method of 2, 6-di-O-methyl-beta-cyclodextrin and inspection method thereof

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preparation example Construction

[0031] The present invention provides a kind of 2,6-di-O-methyl-beta-cyclodextrin industrial mass preparation method, such as figure 1 and figure 2 shown, including the following steps:

[0032] S1: Dry the β-cyclodextrin before feeding, the temperature is controlled at 90°C-130°C, the drying time is 2-15 hours, and the water loss rate is 3%-20%.

[0033] S2: Add anhydrous barium oxide, barium hydroxide, and N,N-dimethylformamide in turn to reaction kettle 1, stir well, cool down to +10°C to -10°C and keep; anhydrous barium oxide, barium hydroxide , The mass ratio of N,N-dimethylformamide to β-cyclodextrin is 30:50:(40~70):(10~35), and β-cyclodextrin is added in 1~5 times , with an interval of 5 to 30 minutes between two adjacent times, and continue to stir for 0.5 to 3 hours after adding all of them; then add methyl sulfate dropwise, the mass ratio of methyl sulfate to β-cyclodextrin is 24: (10 to 25), methyl sulfate The ester is divided into 1 to 5 parts on average, each...

Embodiment 1

[0075] This embodiment provides an industrial mass production method of 2,6-di-O-methyl-β-cyclodextrin, comprising the following steps:

[0076] S1: Dry the β-cyclodextrin before feeding, the temperature is controlled at 130°C, the drying time is 2 hours, and the water loss rate is 20%.

[0077] S2: Add anhydrous barium oxide, barium hydroxide, N,N-dimethylformamide in sequence to reaction kettle 1, stir well, cool down to 10°C and keep; anhydrous barium oxide, barium hydroxide, N,N- The mass ratio of dimethylformamide to β-cyclodextrin is 30:50:40:35, and β-cyclodextrin is added in 5 times, with an interval of 5 minutes between two adjacent times, and stirring is continued for 3 hours after all additions are completed; Then add methyl sulfate dropwise, the mass ratio of methyl sulfate to β-cyclodextrin is 24:10, methyl sulfate is divided into 5 parts on average, each part is added dropwise for 1.5 hours, and stirred for 60 minutes; after all the drops are completed, continue ...

Embodiment 2

[0084] This embodiment provides an industrial mass production method of 2,6-di-O-methyl-β-cyclodextrin, comprising the following steps:

[0085] S1: Dry the β-cyclodextrin before feeding, the temperature is controlled at 90°C, the drying time is 15 hours, and the water loss rate is 3%.

[0086] S2: Add anhydrous barium oxide, barium hydroxide, and N,N-dimethylformamide in turn to reaction kettle 1, stir well, cool down to -10°C and keep; anhydrous barium oxide, barium hydroxide, N,N - The mass ratio of dimethylformamide to β-cyclodextrin is 30:50:70:10, and β-cyclodextrin is added in 2 times, with an interval of 30 minutes between two adjacent times. After all additions, continue stirring for 0.5 h; then add methyl sulfate dropwise, the mass ratio of methyl sulfate to β-cyclodextrin is 24:25, methyl sulfate is divided into 2 parts on average, each part is added dropwise in 4 hours, and stirred for 15 minutes; after all the drops are completed The stirring reaction was continu...

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Abstract

The invention relates to an industrial preparation method of 2, 6-di-O-methyl-beta-cyclodextrin and an inspection method thereof. The method comprises the following steps: S1, drying beta-cyclodextrinbefore feeding; S2: under the condition of low temperature, fully mixing and stirring anhydrous barium oxide, barium hydroxide and N, N-dimethylformamide; then adding the dried beta-cyclodextrin andstirring, then dropping methyl sulfate and stirring, continuously stirring for a preset time after the dropping is finished; S3, closing a low-temperature system in S2, continuously stirring and heating to 20-30 DEG C, and keeping the temperature for continuous reaction for 20-60 hours; S4, extracting the product in S3 by using trichloromethane and then neutralizing; S5, sequentially carrying outsalt washing and water washing on the neutralized product, carrying out suction filtration and collecting the filtrate; S6, dehydrating the filtrate, and then distilling and concentrating the filtrateuntil the filtrate is thick; S7: drying the concentrated solution and recrystallizing to obtain the target product 2, 6-di-o-methyl-beta-cyclodextrin.

Description

technical field [0001] The invention relates to the technical field of synthesis of organic polymer compounds, in particular to an industrial preparation method of 2,6-di-O-methyl-β-cyclodextrin and an inspection method thereof. Background technique [0002] [2,6-Di-O-methyl] 7 -β-cyclodextrin, Heptakis(2,6-di-o-methyl)-β-cyclodextrin is the standard name of the product, which can be abbreviated as 2,6-di-O-methyl-β-cyclodextrin Ethyl or 2,6-di-O-methyl-β-cyclodextrin, some foreign language materials are abbreviated as 2,6-di-o-methyl-β-cyclodextrin, and the molecular formula is C 56 h 98 o 35 , molecular weight 1331.36, appearance is white powder, chemical structure formula is as follows: [0003] [0004] 2,6-Di-O-methyl-β-cyclodextrin is a product obtained by directional methylation reaction with β-cyclodextrin as the main raw material. β-Cyclodextrins (β-Cyclodextrins), abbreviated as β-CD, are formed by condensation and cyclization of seven D-glucopyranose in a ...

Claims

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Application Information

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IPC IPC(8): C08B37/16G01N31/12
Inventor 马文革马越
Owner 廊坊兴龙生物技术有限公司
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