AU2018100420A4 - Organic synthesis raw materials valeric acid synthesis method - Google Patents
Organic synthesis raw materials valeric acid synthesis method Download PDFInfo
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- AU2018100420A4 AU2018100420A4 AU2018100420A AU2018100420A AU2018100420A4 AU 2018100420 A4 AU2018100420 A4 AU 2018100420A4 AU 2018100420 A AU2018100420 A AU 2018100420A AU 2018100420 A AU2018100420 A AU 2018100420A AU 2018100420 A4 AU2018100420 A4 AU 2018100420A4
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- valeric acid
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
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- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
Abstract Organic synthesis raw materials valeric acid synthesis method, comprises the following steps: 3 mol methyl propyl ketone, 4-6 mol tributyl citrate solution were 5 added to the reaction vessel, controlled the stirring speed at 190-220 rpm, the solution temperature was reduced to 6-9 C for 60-80 min, and then the solution temperature was raised to 10-15 'C, added 3-4 mol chromium acetate by 3-6 times, interval for 30-40 min each time, continued to react for 2-3 h, and then standing for 60-80 min, added 300 ml potassium nitrate solution, standing for solution layer, the water layer 10 extracted with 4-heptanone solution by 3-5 times, extracted with 3-methyl-2 pentanone solution by 4-6 times, combined with the oil layer and extraction, recrystallized in the isobutyl butyrate solution, dehydrated with dehydration, got the finished valeric acid .
Description
FIELD OF THE INVENTION
The present invention relates to organic synthesis raw materials valeric acid 5 synthesis method.
GENERAL BACKGROUND
Valeric acid is mainly used for the production of valerate, as spices raw materials and estrogen estradiol valerate and disinfectant raw materials, However, most of the existing synthetic methods are using that formic acid reacts with 1-butene to form n-valeric acid, it is complicated and the final yield is not very high. Therefore, it is necessary to propose a new synthetic method for further improving the quality and yield of the product and reducing the byproduct content, it has important economic significance.
SUMMARY
The purpose of the present invention is to provide organic synthesis raw materials valeric acid synthesis method, comprises the following steps:
(i) 3 mol methyl propyl ketone, 4-6 mol tributyl citrate solution were added to the reaction vessel, controlled the stirring speed at 190-220 rpm, the solution temperature was reduced to 6-9 °C for 60-80 min, and then the solution temperature was raised to 10-15 °C, added 3-4 mol chromium acetate by 3-6 times, interval for 30-40 min each time, continued to react for 2-3 h, and then standing for 60-80 min, added 300 ml potassium nitrate solution, standing for solution layer, the water layer extracted with
4-heptanone solution by 3-5 times, extracted with 3-methyl-2- pentanone solution by 4-6 times, combined with the oil layer and extraction, recrystallized in the isobutyl butyrate solution, dehydrated with dehydration, got the finished valeric acid ;wherein, the mass fraction of the tributyl citrate solution in step (i) is 70 to 78%, the mass fraction of the potassium nitrate solution described in step (i) is 20 to 26%, the mass fraction of the 4-heptanone solution in step (i) is 70-75%, the mass fraction of the
2018100420 01 Apr 2018
3-methy 1-2-pentanone solution described in step (i) is 80-88%, the mass fraction of isobutyl butyrate solution in step (i) is 90-96%.
Throughout the reaction process can be the following reaction formula:
h3ch2chjC^ h3ch,ch2c^ /Oh c + CJSHJ2O7 + C6IIi>O6C] -► jj
O 0
Advantage of the present invention is that: reducing intermediate links reaction, decreasing the reaction time and improving the reaction yield.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
The following examples with reference to specific embodiments of the present invention are further illustrated:
organic synthesis raw materials valeric acid synthesis method.
Embodiment 1 mol methyl propyl ketone, 4 mol tribntyl citrate solution with a mass fraction of
70% were added to the reaction vessel, controlled the stirring speed at 190 rpm, the solution temperature was reduced to 6°C for 60 min, and then the solution temperature was raised to 10 'C, added 3mol chromium acetate by 3 times, interval for 30 min each time, continued to react for 2 h, and then standing for 60 min, added 300 ml potassium nitrate solution with a mass fraction of 20%, standing for solution layer, the water layer extracted with 4-hcptanone solution with a mass fraction of 70% by 3 times, extracted with 3-mcthyl-2- pentanone solution with a mass fraction of 80% by 4 times, combined with the oil layer and extraction, recrystallizcd in the isobutyl butyrate solution with a mass fraction of 90%, dehydrated with anhydrous magnesium sulfatedc dehydration, got the finished valeric acid 240.24g,yield of 91 %.
Embodiment 2 mol methyl propyl ketone, 5 mol tributyl citrate solution with a mass fraction of 75% were added to the reaction vessel, controlled the stirring speed at 210 rpm. the
2018100420 01 Apr 2018 solution temperature was reduced to 7 °C for 70 min, and then the solution temperature was raised to 12 °C, added 3.5mol chromium acetate by 5 times, interval for 35 min each time, continued to react for 2.5 h, and then standing for 70 min, added 300 ml potassium nitrate solution with a mass fraction of 23%, standing for solution layer, the water layer extracted with 4-heptanone solution with a mass fraction of 72% by 4 times, extracted with 3-methyl-2- pentanone solution with a mass fraction of 85% by 5 times, combined with the oil layer and extraction, recrystallized in the isobutyl butyrate solution with a mass fraction of 93%, dehydrated with anhydrous potassium carbonate dehydration, got the finished valeric acid 245.52g,yield of 93%.
Embodiment 3 mol methyl propyl ketone, 6 mol tributyl citrate solution with a mass fraction of 78% were added to the reaction vessel, controlled the stirring speed at 220 rpm, the solution temperature was reduced to 9°C for 80 min, and then the solution temperature was raised to 15 °C, added 4mol chromium acetate by 6 times, interval for 40 min each time, continued to react for 3 h, and then standing for 80 min, added 300 ml potassium nitrate solution with a mass fraction of 26%, standing for solution layer, the water layer extracted with 4-heptanone solution with a mass fraction of 75% by 5 times, extracted with 3-methyl-2- pentanone solution with a mass fraction of 88% by 6 times, combined with the oil layer and extraction, recrystallized in the isobutyl butyrate solution with a mass fraction of 96%, dehydrated with anhydrous magnesium sulfatede hydration, got the finished valeric acid 253.44g,yield of 96%.
2018100420 01 Apr 2018
Claims (3)
- Claims1. Organic synthesis raw materials valeric acid synthesis method, comprises the following steps:(i) 3 mol methyl propyl ketone, 4-6 mol tributyl citrate solution were added to 5 the reaction vessel, controlled the stirring speed at 190-220 rpm, the solution temperature was reduced to 6-9 °C for 60-80 min, and then the solution temperature was raised to 10-15 °C, added 3-4 mol chromium acetate by 3-6 times, interval for 30-40 min each time, continued to react for 2-3 h, and then standing for 60-80 min, added 300 ml potassium nitrate solution, standing for solution layer, the water layer10 extracted with 4-heptanone solution by 3-5 times, extracted with 3-methyl-2pentanone solution by 4-6 times, combined with the oil layer and extraction, recrystallized in the isobutyl butyrate solution, dehydrated with dehydration, got the finished valeric acid ;wherein , the mass fraction of the tributyl citrate solution in step (i) is 70 to 78%, the mass fraction of the potassium nitrate solution described in step (i)15 is 20 to 26%, the mass fraction of the 4-heptanone solution in step (i) is 70-75%.
- 2. Organic synthesis raw materials valeric acid synthesis method according to claim 1 wherein the mass fraction of the 3-methyl-2-pentanone solution described in step (i) is 80-88%.
- 3. Organic synthesis raw materials valeric acid synthesis method according to claim 1 wherein the mass fraction of isobutyl butyrate solution in step (i) is 90-96%.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710215444.0A CN108238891A (en) | 2017-04-05 | 2017-04-05 | A kind of synthetic method of organic synthesis raw material valeric acid |
| CN2017102154440 | 2017-04-05 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| AU2018100420A4 true AU2018100420A4 (en) | 2018-05-10 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| AU2018100420A Ceased AU2018100420A4 (en) | 2017-04-05 | 2018-04-01 | Organic synthesis raw materials valeric acid synthesis method |
Country Status (4)
| Country | Link |
|---|---|
| CN (1) | CN108238891A (en) |
| AU (1) | AU2018100420A4 (en) |
| GB (1) | GB201708116D0 (en) |
| IE (1) | IES86975B2 (en) |
-
2017
- 2017-04-05 CN CN201710215444.0A patent/CN108238891A/en active Pending
- 2017-05-22 GB GBGB1708116.7A patent/GB201708116D0/en not_active Ceased
-
2018
- 2018-03-27 IE IES20180081A patent/IES86975B2/en unknown
- 2018-04-01 AU AU2018100420A patent/AU2018100420A4/en not_active Ceased
Also Published As
| Publication number | Publication date |
|---|---|
| GB201708116D0 (en) | 2017-07-05 |
| IES20180081A2 (en) | 2019-04-03 |
| IES86975B2 (en) | 2019-05-01 |
| CN108238891A (en) | 2018-07-03 |
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