CN100375751C - Production method of prednisone hydrolysate - Google Patents
Production method of prednisone hydrolysate Download PDFInfo
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- CN100375751C CN100375751C CNB2005100162295A CN200510016229A CN100375751C CN 100375751 C CN100375751 C CN 100375751C CN B2005100162295 A CNB2005100162295 A CN B2005100162295A CN 200510016229 A CN200510016229 A CN 200510016229A CN 100375751 C CN100375751 C CN 100375751C
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- hydrolysate
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Abstract
The present invention relates to a technical method for producing prednisone hydrolysate, which comprises the following steps: using prednisone acetate (intermediate body) as raw material, a chloroform methanol mixing solvent as a solvent and a potassium hydroxide solution as catalyst for a reaction at low temperature; neutralizing, concentrating and crystallizing a product after the reaction is finished; cooling, filtering and drying the product to obtain the prednisone hydrolysate. The technical method can enhance the yield and the quality of the prednisone hydrolysate.
Description
Technical field:
The present invention relates to the producing and manufacturing technique of prednisone hydrolysate.
Background technology:
The producing and manufacturing technique of traditional prednisone hydrolysate, as solvent, solid potassium hydroxide is as catalyzer with single solvent methyl alcohol, and 24-26 ℃ of reaction after reaction finishes, neutralizes, condensing crystal, cooling is filtered, and drying gets prednisone hydrolysate.Its shortcoming is that the required solvent amount of single solvent is big, and the quality of reactant and yield are not high.
Summary of the invention:
The present invention is directed to the problem that prior art exists, a kind of producing and manufacturing technique of prednisone hydrolysate is provided, with chloroform: methyl alcohol is solvent, and potassium hydroxide/methyl alcohol is catalyzer, and low temperature reacts, and product quality and yield are improved.
In order to realize purpose of the present invention, provide following technical scheme:
A kind of producing and manufacturing technique of prednisone hydrolysate is characterized in that, with its proportion be 1.10～1.15 chloroform methanol mixed solvents as solvent,, potassium hydroxide solution is as catalyzer, low temperature 0-5 ℃ is reacted.
With chloroform: methyl alcohol (proportion is 1.10～1.15) is solvent, and 4～6% potassium hydroxide/methyl alcohol is catalyzer, and 0～5 ℃ is reacted, after reaction finishes, neutralization, condensing crystal, cooling is filtered, drying, product.
Excellent effect of the present invention can be confirmed by following experimental result.
| Numbering | Charging capacity (g) | Producing and manufacturing technique | Output (g) | Yield (%) | Improve (%) | Content (%) |
| 1 | 60 | New technology | 50 | 83.3 | 8.2 | 97.8 |
| 2 | 60 | New technology | 50.2 | 83.7 | 8.7 | 98.2 |
| 3 | 60 | New technology | 50.5 | 84.2 | 9.4 | 98.2 |
| 4 | 60 | New technology | 50.3 | 83.8 | 8.8 | 98 |
| 5 | 60 | New technology | 50.4 | 84 | 9.1 | 98.1 |
| 6 | 60 | New technology | 50.8 | 84.7 | 10 | 97.9 |
Annotate: yield %=output/charging capacity * 100%
Improve yield %=(new technology yield-existing technology yield)/existing technology yield * 100%
As can be seen from the above table, novel process all is improved product quality and yield in the superiority that has demonstrated him aspect quality and the yield really.
Embodiment:
Embodiment 1:
Throw the 60g raw material, 600～650ml rises chloroform methanol (proportion 1.10～1.15), molten clearly after, adding 4～6% potassium hydroxide/methyl alcohol is catalyzer, and 0～5 ℃ was reacted 30 minutes, after reaction finishes, neutralization, condensing crystal, cooling is filtered, dry, get prednisone hydrolysate 50g, Liquid Detection content is 97.8%, and yield is 83.3%.
Embodiment 2:
Throw the 60g raw material, 600～650ml rises chloroform methanol (proportion 1.10～1.15), molten clearly after, adding 4～6% potassium hydroxide/methyl alcohol is catalyzer, and 0～5 ℃ was reacted 30 minutes, after reaction finishes, neutralization, condensing crystal, cooling is filtered, dry, get prednisone hydrolysate 50.2g, Liquid Detection content is 98.2%, and yield is 83.7%.
Embodiment 3:
Throw the 60g raw material, 600～650ml rises chloroform methanol (proportion 1.10～1.15), molten clearly after, adding 4～6% potassium hydroxide/methyl alcohol is catalyzer, and 0～5 ℃ was reacted 30 minutes, after reaction finishes, neutralization, condensing crystal, cooling is filtered, dry, get prednisone hydrolysate 50.5g, Liquid Detection content is 98.2%, and yield is 84.2%.
Embodiment 4:
Throw the 60g raw material, 600～650ml rises chloroform methanol (proportion 1.10～1.15), molten clearly after, adding 4～6% potassium hydroxide/methyl alcohol is catalyzer, and 0～5 ℃ was reacted 30 minutes, after reaction finishes, neutralization, condensing crystal, cooling is filtered, dry, get prednisone hydrolysate 50.3g, Liquid Detection content is 98%, and yield is 83.8%.
Embodiment 5:
Throw the 60g raw material, 600～650ml rises chloroform methanol (proportion 1.10～1.15), molten clearly after, adding 4～6% potassium hydroxide/methyl alcohol is catalyzer, and 0～5 ℃ was reacted 30 minutes, after reaction finishes, neutralization, condensing crystal, cooling is filtered, dry, get prednisone hydrolysate 50.4g, Liquid Detection content is 98.1%, and yield is 84%.
Embodiment 6:
Throw the 60g raw material, 600～650ml rises chloroform methanol (proportion 1.10～1.15), molten clearly after, adding 4～6% potassium hydroxide/methyl alcohol is catalyzer, and 0～5 ℃ was reacted 30 minutes, after reaction finishes, neutralization, condensing crystal, cooling is filtered, dry, get prednisone hydrolysate 50.8g, Liquid Detection content is 97.9%, and yield is 84.7%.
The prednisone hydrolysate molecular formula is as follows
Claims (1)
1. the producing and manufacturing technique of a prednisone hydrolysate is characterized in that: with proportion be 1.10～1.15 chloroform and methanol mixed solvent as solvent, concentration be 4%～6% potassium hydroxide and methanol solution as catalyzer, low temperature 0-5 ℃ is reacted.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100162295A CN100375751C (en) | 2005-02-24 | 2005-02-24 | Production method of prednisone hydrolysate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100162295A CN100375751C (en) | 2005-02-24 | 2005-02-24 | Production method of prednisone hydrolysate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1824670A CN1824670A (en) | 2006-08-30 |
| CN100375751C true CN100375751C (en) | 2008-03-19 |
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| Application Number | Title | Priority Date | Filing Date |
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| CNB2005100162295A Active CN100375751C (en) | 2005-02-24 | 2005-02-24 | Production method of prednisone hydrolysate |
Country Status (1)
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| CN (1) | CN100375751C (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102617686A (en) * | 2012-03-16 | 2012-08-01 | 浙江凯迪药业有限公司 | Preparation method of prednisone |
| CN103087135A (en) * | 2013-01-17 | 2013-05-08 | 河南利华制药有限公司 | Hydrolysis preparation technology of prednisone |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1361108A (en) * | 2000-12-27 | 2002-07-31 | 天津药业集团有限公司 | Production process of prednisolone Acetate condensating reduced product |
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2005
- 2005-02-24 CN CNB2005100162295A patent/CN100375751C/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1361108A (en) * | 2000-12-27 | 2002-07-31 | 天津药业集团有限公司 | Production process of prednisolone Acetate condensating reduced product |
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| Publication number | Publication date |
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| CN1824670A (en) | 2006-08-30 |
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Address after: 300161 No. 19, Xinye 9th Street, West District, Binhai New Area Development Zone, Tianjin Patentee after: TIANJIN TIANYAO PHARMACEUTICAL Co.,Ltd. Address before: Cheng linzhuan Hedong District of Tianjin City Road 300161 No. 91 Patentee before: TIANJIN TIANYAO PHARMACEUTICAL Co.,Ltd. |
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Address after: 300161 No. 19, Xinye 9th Street, West District, Binhai New Area Development Zone, Tianjin Patentee after: Tianjin Pharmaceutical Co.,Ltd. Address before: 300161 No. 19, Xinye 9th Street, West District, Binhai New Area Development Zone, Tianjin Patentee before: TIANJIN TIANYAO PHARMACEUTICAL Co.,Ltd. |
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