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Preparation method for glucocorticoid 20-ketal intermediate product

A technology of glucocorticoids and ketals, which is applied in the field of biomedicine, can solve the problems of low reaction conversion rate of intermediates and non-reusable catalysts, and achieve the effects of increasing yield, reducing impurities, and reducing costs

Inactive Publication Date: 2011-05-11
GUANGXI WANDE PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The use of organic acids as catalysts has the following disadvantages: the catalyst cannot be reused, the conversion rate of the intermediate reaction is low, and it needs to be neutralized with alkali after the reaction is completed.

Method used

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  • Preparation method for glucocorticoid 20-ketal intermediate product
  • Preparation method for glucocorticoid 20-ketal intermediate product
  • Preparation method for glucocorticoid 20-ketal intermediate product

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] 1. Raw materials

[0056] Glucocorticoid ketal precursor 90kg

[0057] Ethyl acetate 600L

[0058] Ethylene glycol 90L

[0059] Triethyl orthoformate 80L

[0060] H Y molecular sieve 10kg

[0061] 2. Preparation method steps and conditions

[0062] Add 600L of ethyl acetate, 90L of ethylene glycol, 80L of triethyl orthoformate, and 90kg of glucocorticoid ketal precursors into the reaction kettle, stir, and add 10kg of HY molecular sieve catalyst. Heat to reflux for 2 hours, filter and separate molecular sieves, concentrate and recover ethyl acetate with a remaining volume of about 240L, cool to 0-5°C, stir for 1 hour, filter, and dry the filter cake in a hot air stream at 80°C. Get dry 94.1kg, detect and meet quality regulation, yield (molar yield): 92.4%

Embodiment 2

[0064] 1. Raw materials

[0065] Glucocorticoid ketal precursor 90kg

[0066] Ethyl acetate 600L

[0067]Ethylene glycol 90L

[0068] Triethyl orthoformate 60L

[0069] H Y molecular sieve 15kg

[0070] 2. Preparation method steps and conditions

[0071] Add 600L of ethyl acetate, 90L of ethylene glycol, 60L of triethyl orthoformate, and 90kg of glucocorticoid ketal precursors into the reaction kettle, stir, and add 15kg of HY molecular sieve catalyst. Heat to reflux for 3 hours, filter to separate molecular sieves, concentrate and recover ethyl acetate with a remaining volume of about 240L, cool to 0-5°C, stir for 1 hour, filter, and dry the filter cake in a hot air stream at 80°C. Get dry 94.5kg, detect and meet quality regulation, yield (molar yield): 92.8%

Embodiment 3

[0073] 1. Raw materials

[0074] Glucocorticoid ketal precursor 90kg

[0075] Toluene 400L

[0076] Ethylene glycol 90L

[0077] Triethyl orthoformate 120L

[0078] H Y molecular sieve 20kg

[0079] 2. Preparation method steps and conditions

[0080] Add 400L of toluene, 90L of ethylene glycol, 120L of triethyl orthoformate, and 90kg of glucocorticoid ketal precursors into the reaction kettle, stir, and add 20kg of H Y molecular sieve catalyst. Heat to reflux for 2 hours, filter to separate molecular sieves, concentrate and recover ethyl acetate with a remaining volume of about 180L, cool to 0-5°C, stir for 1 hour, filter, and dry the filter cake in a hot air stream at 80°C. Get dry 94.8kg, detect and meet quality regulation, yield (molar yield): 93.1%

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Abstract

The invention relates to a preparation method for a glucocorticoid 20-ketal intermediate product, which comprises the steps of respectively adding organic solvents of acetic ether, toluene, glycol, ethyl ortho formate and a glucocorticoid ketal precursor into a reaction container, stirring, adding H Y molecular sieve catalyst according to a weight ratio of H Y molecular sieve: glucocorticoid 20-ketal precursor being equal to 1.0:0.1 to 0.5, reflowing for 2 hours, cooling to room temperature, filtering and separating the H Y molecular sieve, conducting concentration and distillation to obtain crystals separated out from the organic solvents, filtering, separating and drying. As the catalyst, the H Y molecular sieve can be reused, thereby reducing environmental pollution and increasing the yield of the glucocorticoid 20-ketal intermediate product by 6 to 8 percent.

Description

technical field [0001] The invention relates to the field of biomedicine, in particular to a method for preparing a glucocorticoid 20-ketal intermediate. Background technique [0002] The glucocorticoid 20-ketal intermediate is an intermediate in the production of glucocorticoid drugs. The existing production process is mainly to condense the glucocorticoid 20-ketal precursor with ethylene glycol at the 20-position The organic acid catalyst commonly used in ketone reaction and ketal reaction is p-aminobenzoic acid. After the ketal reaction, distill off the water, reflux for 6-10 hours, add alkali to neutralize the organic acid, distill and concentrate the reaction liquid to crystallize, filter and separate, and dry. The specific experimental method step is to add 300ml ethyl acetate, 45ml ethylene glycol, and 40ml triethyl orthoformate into the reaction flask respectively, stir, and add 0.9g p-toluenesulfonic acid. Keep at 25-30°C, add 45g of glucocorticoid 20-ketal precurs...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07J71/00
CPCY02P20/584
Inventor 梁宇坚杨冰吕明航李大宁
Owner GUANGXI WANDE PHARMA