Method for recycling betamethasone or dexamethasone synthetic mother liquor materials

A technology of dexamethasone and betamethasone, which is applied in the production of steroids, bulk chemicals, organic chemistry, etc., and can solve the problems of waste of polluted materials, excessive tar, and failure to recycle, etc.

Active Publication Date: 2020-02-28
HUNAN NORCHEM PHARMACEUTICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the current production process, the mother liquid material is basically unable to be recycled due to its high impurity content and tar content. After concentration, it will be treated as solid waste, causing pollution and a great waste of materials.

Method used

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  • Method for recycling betamethasone or dexamethasone synthetic mother liquor materials
  • Method for recycling betamethasone or dexamethasone synthetic mother liquor materials
  • Method for recycling betamethasone or dexamethasone synthetic mother liquor materials

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054]

[0055] Collect 2000mL of the masterbatch solution of betamethasone produced in the above fluorine synthesis step, concentrate under reduced pressure until there is no fraction, add dichloromethane and heat to reflux, add 100g of silica gel and stir for 1h, filter, collect the filtrate, concentrate to a small volume, Add 200 mL of ethyl acetate to replace, concentrate to a paste, cool to room temperature, and filter to obtain a brown solid, which is dried to obtain 45 g of solid 1a (shown below), with a purity of 71%. After further column chromatography purification, the structure was determined to be 1a structure, MS-ESI (m / z): 375.2[M+H] + , 1 HNMR (400MHz, DMSO d6 ):δ9.62(s,1H),7.71(s,1H),7.29(d,J=10.4,1H),6.20-6.23(m,1H),6.01(s,1H),5.40-5.42(m ,1H),4.07-4.10(m,1H),3.34-3.32(m,2H),2.32-2.66(m,4H),1.86-2.00(m,2H),1.19-1.52(m,12H)

[0056] 1) Protective reaction:

[0057]

[0058] In a three-neck flask, add 30g of the above solid 1a, 150mL of dichloromethane, ...

Embodiment 2

[0065]

[0066] Collect 2000 mL of the dexamethasone masterbatch solution after the above fluorine synthesis step, concentrate under reduced pressure until there is no fraction, add ethyl acetate and heat to reflux, add 100 g of silica gel and stir for 1 hour, filter, collect the filtrate, concentrate to a small volume, Cool down to room temperature for crystallization, filter to obtain a yellow solid, and dry to obtain 33 g of solid 1b with a purity of 76%.

[0067] 1) Protective reaction:

[0068]

[0069] In the three-necked flask, add 30g of solid 1b, 100mL of DMF, 10g of potassium carbonate and 30mL of dimethyl carbonate, the reaction temperature is raised to 80-85°C for 2-3h, the dimethyl carbonate and part of the DMF are concentrated under reduced pressure, and then the system is poured into into 300mL of ice water, stirred evenly, and filtered to obtain the wet product of compound 2b-2, which was directly used in the next reaction.

[0070] 2) Reduction reaction...

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Abstract

The invention relates to a method for recycling betamethasone or dexamethasone synthetic mother liquor materials. The method comprises the following steps: extracting a compound shown as formula 1 from a mother liquor material; carrying out protection reaction of the 20th site hydroxyl group on the compound shown as formula 1 to obtain a compound shown as formula 2; carrying out a reduction reaction of the 21th site aldehyde group on the compound shown as formula 2 to obtain a compound shown as formula 3, and continuously carrying out oxidation reaction and hydrolysis reaction to obtain a compound shown as 4 which is betamethasone or dexamethasone. The above recycling method can convert the betamethasone or dexamethasone mother liquor material into betamethasone or dexamethasone with highmedicinal value and economic benefit, and huge economic benefit is achieved.

Description

technical field [0001] The invention relates to the technical field of pharmaceutical synthesis, in particular to a method for recycling betamethasone or dexamethasone synthesis mother liquor. Background technique [0002] The final step in the synthesis process of betamethasone and dexamethasone is all fluorine reaction, and the reaction is carried out in hydrofluoric acid. Taking the synthesis process of betamethasone as an example, the reaction formula is as follows. [0003] [0004] Because the above-mentioned reaction is carried out in high-concentration hydrofluoric acid, a lot of by-products are inevitably generated in the reaction process, and the molar yield of dexamethasone and betamethasone after refining and purification is only about 80% to 85%. The impurity entered in the mother liquor material of dexamethasone and betamethasone synthesis. In the current production process, the mother liquid material is basically unable to be recycled due to its high impu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J5/00
CPCC07J5/0076Y02P20/55
Inventor 唐杰曾春玲邹元
Owner HUNAN NORCHEM PHARMACEUTICAL CO LTD
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