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Industrial preparation method of 2,6-di-o-methyl-β-cyclodextrin and its inspection method

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

Active Publication Date: 2021-06-01
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-β-cyclodextrin and its inspection method
  • Industrial preparation method of 2,6-di-o-methyl-β-cyclodextrin and its inspection method
  • Industrial preparation method of 2,6-di-o-methyl-β-cyclodextrin and its inspection method

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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-β-cyclodextrin and an inspection method thereof, comprising steps: S1: drying the β-cyclodextrin before feeding; S2 : Under low temperature conditions, mix anhydrous barium oxide, barium hydroxide and N,N-dimethylformamide and stir thoroughly; then add dried β-cyclodextrin and stir, then add methyl sulfate dropwise and stir, and continue to stir for the preset time after all the drops are completed; S3: close the low-temperature system in S2 and continue stirring to raise the temperature to 20-30°C, keep the temperature and continue the reaction for 20-60h; S4: use the product of S3 with chloroform Neutralize after extraction; S5: Wash the neutralized product with salt and water in turn, suction filter and collect the filtrate; S6: Dehydrate the filtrate, then distill and concentrate until the filtrate is concentrated to viscous; S7: Dry the concentrate, After recrystallization, the target product 2,6-two-O-methyl-β-cyclodextrin was obtained.

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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Patent Type & Authority Patents(China)
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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