CN102603530A - Production method of fluoro-methyl propionlyacetae - Google Patents
Production method of fluoro-methyl propionlyacetae Download PDFInfo
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- CN102603530A CN102603530A CN2012100386898A CN201210038689A CN102603530A CN 102603530 A CN102603530 A CN 102603530A CN 2012100386898 A CN2012100386898 A CN 2012100386898A CN 201210038689 A CN201210038689 A CN 201210038689A CN 102603530 A CN102603530 A CN 102603530A
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- fluoro
- methyl acetate
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- reaction kettle
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Abstract
The invention discloses a production method of fluoro-methyl propionlyacetae, comprising the following steps: adding methyl fluoroacetate and ethyl propionate solvent at a weight ratio of 1:3 into a reaction kettle; adding metal sodium; after metal sodium is added, holding at 25-35 DEG C for 3-4 hours and transferring into an acylation kettle; cooling to 20 DEG C; dropwise adding propionyl chloride; holding the temperature for 2-3 hours and transferring into a desolvation distillation kettle; distilling out the solvent and the fluoro-methyl propionlyacetae product; delivering residual solid waste to a solid waste collecting place; and recycling the distilled solvent. The production method provided by the invention is simple and convenient, easy in operation and high in product yield; before rectification, the crude product yield is up to above 88%, the product content is up to above 92%, and the finished product yield is up to above 85%; and after rectification, the rectification yield is up to above 95%, and the finished product content can be up to above 98%.
Description
Technical field
The present invention relates to a kind of working method of fluoro propionyl methyl acetate.
Background technology
The working method of existing fluoro propionyl methyl acetate is complicated, and the product yield is low, and finished product content is low.
Summary of the invention
The object of the present invention is to provide a kind of easy to operately, yield is high, the working method of the fluoro propionyl methyl acetate that finished product content is high.
Technical solution of the present invention is:
A kind of working method of fluoro propionyl methyl acetate is characterized in that: methylfluoracetate and solvent ethyl propionate dropped into reaction kettle by weight 1:3, opens and stir,, advance kerosene in the chuck of reaction kettle, control kerosene temperature is at 25 ~ 30 ℃; Open oxygen meter and also in reaction kettle, feed oxygen level≤4% in nitrogen to the still, begin to drop into sodium Metal 99.5 then, after adding sodium and finishing; 25 ~ 30 ℃ of insulations 3 ~ 4 hours, and change the acidylate still over to, be cooled to 20 ℃; Drip propionyl chloride, be incubated 2 ~ 3 hours then, change the precipitation still kettle over to; Steam solvent and product fluoro propionyl methyl acetate, the residual solid waste residue send useless admittedly collection place, the solvent recuperation utilization that steams.
Sodium Metal 99.5 repeatedly adds, and each add-on is identical, and the sodium Metal 99.5 add-on is 10 ~ 25% of a methylfluoracetate weight.
30 ~ 45% of the consumption methylfluoracetate weight of propionyl chloride.
The cut that contains product fluoro propionyl methyl acetate gets into rectifying tower rectifying, obtains finished product.
The inventive method is easy, and is easy to operate, and product yield is high, and the bullion yield before the rectifying reaches more than 88%, and product content is more than 92%, and the finished product yield is more than 85%; Rectifying yield after the rectifying reaches more than 95%, and finished product content can reach more than 98%.
Below in conjunction with embodiment the present invention is described further.
Embodiment
A kind of working method of fluoro propionyl methyl acetate drops into reaction kettle with methylfluoracetate and solvent ethyl propionate by weight 1:3, and open and stir,, advance kerosene in the chuck of reaction kettle, control kerosene temperature is at 25 ~ 30 ℃; Open oxygen meter and also in reaction kettle, feed oxygen level≤4% in nitrogen to the still, begin to drop into sodium Metal 99.5 then, after adding sodium and finishing; 25 ~ 30 ℃ of insulations 3 ~ 4 hours, and change the acidylate still over to, be cooled to 20 ℃; Drip propionyl chloride, be incubated 2 ~ 3 hours then, change the precipitation still kettle over to; Steam solvent and product fluoro propionyl methyl acetate, the residual solid waste residue send useless admittedly collection place, the solvent recuperation utilization that steams.
Sodium Metal 99.5 repeatedly adds, and each add-on is identical, and the sodium Metal 99.5 add-on is 15% of a methylfluoracetate weight.
30 ~ 45% (examples 30%, 40%, 45%) of the consumption methylfluoracetate weight of propionyl chloride.The cut that contains product fluoro propionyl methyl acetate gets into rectifying tower by ordinary method rectifying, obtains finished product.
Bullion yield before the rectifying reaches more than 88%, and product content is more than 92%, and the finished product yield is more than 85%; Rectifying yield after the rectifying reaches more than 95%, and finished product content can reach more than 98%.
Claims (4)
1. the working method of a fluoro propionyl methyl acetate is characterized in that: methylfluoracetate and solvent ethyl propionate dropped into reaction kettle by weight 1:3, opens and stir,, advance kerosene in the chuck of reaction kettle, control kerosene temperature is at 25 ~ 30 ℃; Open oxygen meter and also in reaction kettle, feed oxygen level≤4% in nitrogen to the still, begin to drop into sodium Metal 99.5 then, after adding sodium and finishing; 25 ~ 30 ℃ of insulations 3 ~ 4 hours, and change the acidylate still over to, be cooled to 20 ℃; Drip propionyl chloride, be incubated 2 ~ 3 hours then, change the precipitation still kettle over to; Steam solvent and product fluoro propionyl methyl acetate, the residual solid waste residue send useless admittedly collection place, the solvent recuperation utilization that steams.
2. the working method of fluoro propionyl methyl acetate according to claim 1, it is characterized in that: sodium Metal 99.5 repeatedly adds, and each add-on is identical, and the sodium Metal 99.5 add-on is 10 ~ 25% of a methylfluoracetate weight.
3. the working method of fluoro propionyl methyl acetate according to claim 1 and 2 is characterized in that: 30 ~ 45% of the consumption methylfluoracetate weight of propionyl chloride.
4. the working method of fluoro propionyl methyl acetate according to claim 1 and 2 is characterized in that: the cut that contains product fluoro propionyl methyl acetate gets into rectifying tower rectifying, obtains finished product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012100386898A CN102603530A (en) | 2012-02-21 | 2012-02-21 | Production method of fluoro-methyl propionlyacetae |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012100386898A CN102603530A (en) | 2012-02-21 | 2012-02-21 | Production method of fluoro-methyl propionlyacetae |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102603530A true CN102603530A (en) | 2012-07-25 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN2012100386898A Pending CN102603530A (en) | 2012-02-21 | 2012-02-21 | Production method of fluoro-methyl propionlyacetae |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2002051789A1 (en) * | 2000-12-26 | 2002-07-04 | Tosoh F-Tech, Inc. | Processes for preparing 2-fluoro-3-oxoalkylcarboxylic acid esters |
| CN102060784A (en) * | 2009-11-13 | 2011-05-18 | 南通法茵克医药化工有限公司 | Method for synthesizing 6-ethyl-5-fluoro-4-hydroxy pyrimidine and intermediate thereof |
| CN102190628A (en) * | 2010-03-03 | 2011-09-21 | 浙江海翔药业股份有限公司 | Preparation method of 5-fluoro-6-ethyl-4-hydroxypyrimidine intermediate and Voriconazole |
-
2012
- 2012-02-21 CN CN2012100386898A patent/CN102603530A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2002051789A1 (en) * | 2000-12-26 | 2002-07-04 | Tosoh F-Tech, Inc. | Processes for preparing 2-fluoro-3-oxoalkylcarboxylic acid esters |
| CN102060784A (en) * | 2009-11-13 | 2011-05-18 | 南通法茵克医药化工有限公司 | Method for synthesizing 6-ethyl-5-fluoro-4-hydroxy pyrimidine and intermediate thereof |
| CN102190628A (en) * | 2010-03-03 | 2011-09-21 | 浙江海翔药业股份有限公司 | Preparation method of 5-fluoro-6-ethyl-4-hydroxypyrimidine intermediate and Voriconazole |
Non-Patent Citations (3)
| Title |
|---|
| 《Tetrahedron Letters》 19891230 Thenappan, Alagappan et al An expedient synthesis of alpha-fluoro-beta-keto esters 第30卷, 第45期 * |
| THENAPPAN, ALAGAPPAN ET AL: "An expedient synthesis of α-fluoro-β-keto esters", 《TETRAHEDRON LETTERS》 * |
| 吕微巍: "三唑类抗真菌新药伏立康唑的合成工艺优化", 《中国优秀硕士学位论文全文数据库》 * |
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Application publication date: 20120725 |