CN101125826B - Preparation for florfenicol amine - Google Patents
Preparation for florfenicol amine Download PDFInfo
- Publication number
- CN101125826B CN101125826B CN2007101493453A CN200710149345A CN101125826B CN 101125826 B CN101125826 B CN 101125826B CN 2007101493453 A CN2007101493453 A CN 2007101493453A CN 200710149345 A CN200710149345 A CN 200710149345A CN 101125826 B CN101125826 B CN 101125826B
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- China
- Prior art keywords
- florfenicol
- preparation
- amine
- florfenicol amine
- protonic solvent
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Abstract
The invention relates to a florfenicol amine preparation method, which adopts florfenicol as raw material. Florfenicol is firstly processed with alkali, and then salted out, filtered and dried; finally the florfenicol amine is prepared. The method is characterized in that the technology is simple, the product is highly purified without purifying, the yield is high and the preparation cost is low.
Description
Technical field the invention belongs to the field of fluorinated organic compound, and florfenicol amine is important organic intermediate and analytical reagent.
Its synthetic method of background technology such as US4235892 adopt thiamphenicol hydrolysis in the presence of hydrochloric acid get D-Su Shi-1-[(right-methylsulfonyl) phenyl]-1, ammediol, amino with the phthalic anhydride protection again, the diethylin sulfonium triflate is fluoridized, hydrazine hydrate reacts and gets; Complex process, preparation cycle is long.
Summary of the invention is at above-mentioned shortcoming, concentrate on studies, invented adopt florfenicol in the presence of protonic solvent with the alkaline matter effect, saltout, method that filtration, exsiccant prepare florfenicol amine, not only technology is very simple, product is without purification, and purity is quite high, has the yield height, the characteristics that preparation cost is very low.
Reaction equation is as follows:
Embodiment
With florfenicol 53.73g (0.15mol), water 75mL, alkaline matter 6.40g adding is equipped with in the 250mL there-necked flask of reflux exchanger, agitator and thermometer, be stirred to the solution clarification under about 45 ℃, add NaCl 15.00g, restir is to all dissolvings, spend the night after being cooled to room temperature, leach solid, drying obtains white solid 31.49g, mix with standard substance, use high-performance liquid chromatogram determination, its appearance time equally is a same substance, content 98.77% (high performance liquid chromatography).
Claims (3)
1. method for preparing florfenicol amine, it is characterized in that adopting florfenicol in the presence of protonic solvent with the alkaline matter effect, saltout again, filter, drying prepares.
2. claim 1 neutral and alkali material comprises sodium hydroxide, potassium hydroxide, yellow soda ash, sodium bicarbonate.
3. protonic solvent comprises water, methyl alcohol, ethanol, Virahol in the claim 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007101493453A CN101125826B (en) | 2007-09-05 | 2007-09-05 | Preparation for florfenicol amine |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007101493453A CN101125826B (en) | 2007-09-05 | 2007-09-05 | Preparation for florfenicol amine |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101125826A CN101125826A (en) | 2008-02-20 |
| CN101125826B true CN101125826B (en) | 2011-09-28 |
Family
ID=39093978
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2007101493453A Expired - Fee Related CN101125826B (en) | 2007-09-05 | 2007-09-05 | Preparation for florfenicol amine |
Country Status (1)
| Country | Link |
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| CN (1) | CN101125826B (en) |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1869016A (en) * | 2006-07-04 | 2006-11-29 | 福建出入境检验检疫局检验检疫技术中心 | Preparation method of fluoro thiamphenicol metabolite fluoro thiamphenicol amine |
-
2007
- 2007-09-05 CN CN2007101493453A patent/CN101125826B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1869016A (en) * | 2006-07-04 | 2006-11-29 | 福建出入境检验检疫局检验检疫技术中心 | Preparation method of fluoro thiamphenicol metabolite fluoro thiamphenicol amine |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101125826A (en) | 2008-02-20 |
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Granted publication date: 20110928 Termination date: 20120905 |