AU2018100419A4 - Organic intermediates dimethylacetic acid synthesis method - Google Patents
Organic intermediates dimethylacetic acid synthesis method Download PDFInfo
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- AU2018100419A4 AU2018100419A4 AU2018100419A AU2018100419A AU2018100419A4 AU 2018100419 A4 AU2018100419 A4 AU 2018100419A4 AU 2018100419 A AU2018100419 A AU 2018100419A AU 2018100419 A AU2018100419 A AU 2018100419A AU 2018100419 A4 AU2018100419 A4 AU 2018100419A4
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- dimethylacetic 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)
Abstract
Abstract Organic intermediates dimethylacetic acid synthesis method, comprises the following steps: 2 mol 3-bromo-isopentene and 4-6 mol glycerol triacetate were added 5 to the reaction vessel, controlled the stirring speed at 130-170 rpm for 30-50 min, reduced the solution temperature to 7-10"C, then add 3-5 mol vanadium dioxide, reacted for 60-80 min, and then added 1500 ml potassium bromide solution by 3-5 times, interval for 20-30 min each time, reduced the temperature to 3-5 'C, after addition, standing for 2-4h, washed with sodium sulfate solution in 3-5 times, 10 extracted with 3-methoxy propionitrile solution by 4-6 times, extracted with o-dibromobenzene solution by 5-8 times, recrystallized in o-chloroaniline solution, dehydrated with the dehydrating agent, got the finished dimethylacetic acid crystals.
Description
FIELD OF THE INVENTION
The present invention relates to organic intermediates dimethylacetic acid 5 synthesis method.
GENERAL BACKGROLND
Dimethylacetic acid is mainly used for the raw materials of perfume and perfume esters, it is also used as a textile auxiliaries in the form of salts and as a solvent for a variety of chemical reactions. However, most of the existing synthetic methods are using hydrolysis of isobutyronitrile, 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.
SLMMARY
The purpose of the present invention is to provide organic intermediates dimethylacetic acid synthesis method, comprises the following steps:
(i) 2 mol 3-bromo-isopentene and 4-6 mol glycerol triacetate were added to the reaction vessel, controlled the stirring speed at 130-170 rpm for 30-50 min, reduced the solution temperature to 7-10°C, then add 3-5 mol vanadium dioxide, reacted for 60-80 min, and then added 1500 ml potassium bromide solution by 3-5 times, interval for 20-30 min each time, reduced the temperature to 3- 5°C, after addition, standing for 2-4h, washed with sodium sulfate solution in 3-5 times, extracted with 3-methoxy propionitrile solution by 4-6 times, extracted with o-dibromobenzene solution by 5-8 times, recrystallized in o-chloroaniline solution, dehydrated with the dehydrating agent, got the finished dimethylacetic acid crystals; wherein, the mass fraction of the potassium bromide solution in step (i) is 20 to 28%, the mass fraction of the sodium sulfate solution described in step (i) is 10 to 16%, the mass fraction of the
3-methoxypropionitrile solution in step (i) is 70-75%, the mass fraction of the
2018100419 01 Apr 2018 o-dibromobenzene solution described in step (i) is 80-87%, the mass fraction of o-chloroaniline solution in step (i)is 90-96%.
Throughout the reaction process can be the following reaction formula:
Br
I H
H3C .CO Oh y ch2 + C9H,4O6 + Vq2 _CH CH3 CH3
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 intermediates dimethylacetic acid synthesis method.
Embodiment 1 mol 3-bromo-isopentene and 4 mol glycerol triacetate were added to the reaction vessel, controlled the stirring speed at 130rpm for 30 min, reduced the solution temperature to 7°C, then add 3 mol vanadium dioxide, reacted for 60 min, and then added 1500 ml potassium bromide solution with a mass fraction of 20% by 3 times, interval for 20 min each time, reduced the temperature to 3 °C, after addition, standing for 2h, washed with sodium sulfate solution with a mass fraction of 10% in 3 times, extracted with 3-methoxy propionitrile solution with a mass fraction of 70% by 4 times, extracted with o-dibromobenzene solution with a mass fraction of 80% by 5 times, recrystallized in o-chloroaniline solution with a mass fraction of 90%, dehydrated with the anhydrous potassium carbonate dehydrating agent, got the finished dimethylacetic acid crystals 160.16g, yield of 91%.
Embodiment 2 mol 3-bromo-isopentene and 5 mol glycerol triacetate were added to the reaction
2018100419 01 Apr 2018 vessel, controlled the stirring speed at 150rpm for 40 min, reduced the solution temperature to 8°C, then add 4 mol vanadium dioxide, reacted for 70 min, and then added 1500 ml potassium bromide solution with a mass fraction of 24% by 4 times, interval for 25 min each time, reduced the temperature to 4°C, after addition, standing for 3h, washed with sodium sulfate solution with a mass fraction of 13% in 4 times, extracted with 3-methoxy propionitrile solution with a mass fraction of 73% by 5 times, extracted with o-dibromobenzene solution with a mass fraction of 83% by 6 times, recrystallized in o-chloroaniline solution with a mass fraction of 93%, dehydrated with the dehydrating agent, got the finished dimethylacetic acid crystals 163.68g, yield of
93%.
Embodiment 3 mol 3-bromo-isopentene and 6 mol glycerol triacetate were added to the reaction vessel, controlled the stirring speed at 170rpm for 50 min, reduced the solution temperature to 10°C, then add 5 mol vanadium dioxide, reacted for 80 min, and then added 1500 ml potassium bromide solution with a mass fraction of 28% by 5 times, interval for 30 min each time, reduced the temperature to 5°C, after addition, standing for 4h, washed with sodium sulfate solution with a mass fraction of 16% in 5 times, extracted with 3-methoxy propionitrile solution with a mass fraction of 75% by 6 times, extracted with o-dibromobenzene solution with a mass fraction of 87% by 8 times, recrystallized in o-chloroaniline solution with a mass fraction of 96%, dehydrated with the dehydrating agent, got the finished dimethylacetic acid crystals 168.96g, yield of
96%
2018100419 01 Apr 2018
Claims (3)
- Claims1. Organic intermediates dimethylacetic acid synthesis method, comprises the following steps:(i) 2 mol 3-bromo-isopentene and 4-6 mol glycerol triacetate were added to the 5 reaction vessel, controlled the stirring speed at 130-170 rpm for 30-50 min, reduced the solution temperature to 7-10°C, then add 3-5 mol vanadium dioxide, reacted for 60-80 min, and then added 1500 ml potassium bromide solution by 3-5 times, interval for 20-30 min each time, reduced the temperature to 3- 5°C, after addition, standing for 2-4h, washed with sodium sulfate solution in 3-5 times, extracted with 3-methoxy10 propionitrile solution by 4-6 times, extracted with o-dibromobenzene solution by 5-8 times, recrystallized in o-chloroaniline solution, dehydrated with the dehydrating agent, got the finished dimethylacetic acid crystals; wherein, the mass fraction of the potassium bromide solution in step (i) is 20 to 28%, the mass fraction of the sodium sulfate solution described in step (i) is 10 to 16%, the mass fraction of the15 3-methoxypropionitrile solution in step (i) is 70-75%.
- 2. Organic intermediates dimethylacetic acid synthesis method according to claim 1 wherein the mass fraction of the o-dibromobenzene solution described in step (i) is 80-87%.
- 3. Organic intermediates dimethylacetic acid synthesis method according to claim 1 wherein the mass fraction of o-chloroaniline solution in step (i)is 90-96%.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710212780.XA CN108238889A (en) | 2017-04-05 | 2017-04-05 | A kind of synthetic method of organic intermediate dimethyl acetic acid |
| CN201710212780X | 2017-04-05 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| AU2018100419A4 true AU2018100419A4 (en) | 2018-05-10 |
Family
ID=59220737
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| AU2018100419A Ceased AU2018100419A4 (en) | 2017-04-05 | 2018-04-01 | Organic intermediates dimethylacetic acid synthesis method |
Country Status (4)
| Country | Link |
|---|---|
| CN (1) | CN108238889A (en) |
| AU (1) | AU2018100419A4 (en) |
| GB (1) | GB201708115D0 (en) |
| IE (1) | IES86976B2 (en) |
-
2017
- 2017-04-05 CN CN201710212780.XA patent/CN108238889A/en active Pending
- 2017-05-22 GB GBGB1708115.9A patent/GB201708115D0/en not_active Ceased
-
2018
- 2018-03-27 IE IES20180082A patent/IES86976B2/en unknown
- 2018-04-01 AU AU2018100419A patent/AU2018100419A4/en not_active Ceased
Also Published As
| Publication number | Publication date |
|---|---|
| GB201708115D0 (en) | 2017-07-05 |
| CN108238889A (en) | 2018-07-03 |
| IES86976B2 (en) | 2019-05-01 |
| IES20180082A2 (en) | 2019-04-03 |
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| FGI | Letters patent sealed or granted (innovation patent) | ||
| MK22 | Patent ceased section 143a(d), or expired - non payment of renewal fee or expiry |