AU2018100824A4 - Nitro-cotton intermediates butyl butyrate synthesis method - Google Patents
Nitro-cotton intermediates butyl butyrate synthesis method Download PDFInfo
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- AU2018100824A4 AU2018100824A4 AU2018100824A AU2018100824A AU2018100824A4 AU 2018100824 A4 AU2018100824 A4 AU 2018100824A4 AU 2018100824 A AU2018100824 A AU 2018100824A AU 2018100824 A AU2018100824 A AU 2018100824A AU 2018100824 A4 AU2018100824 A4 AU 2018100824A4
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
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- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
- Detergent Compositions (AREA)
- Pyridine Compounds (AREA)
Abstract
Nitro-cotton intermediates butyl butyrate synthesis method Abstract The present invention discloses nitro-cotton intermediates butyl butyrate synthesis method, comprises the following steps: 2-amino-butanone, potassium chloride solution were added to the reaction vessel, raised the temperature of the solution, controlled the stirring speed, reacted, added anisole solution, raised the temperature of the solution, continued to react; added benzyl benzoate solution, ruthenium dioxide powder, raised the stirring speed, continued to react, added sodium sulfate solution, set aside, stratified solution, separated reservoir, washed with the ethyl cyanide solution for several times, washed with the pyridine solution for several times, re-crystallized in the tri-cyclic ethylamine solution, dehydrated with dehydration, got the finished product butyl butyrate. Figure 1
Description
The present invention discloses nitro-cotton intermediates butyl butyrate synthesis method, comprises the following steps: 2-amino-butanone, potassium chloride solution were added to the reaction vessel, raised the temperature of the solution, controlled the stirring speed, reacted, added anisole solution, raised the temperature of the solution, continued to react; added benzyl benzoate solution, ruthenium dioxide powder, raised the stirring speed, continued to react, added sodium sulfate solution, set aside, stratified solution, separated reservoir, washed with the ethyl cyanide solution for several times, washed with the pyridine solution for several times, re-crystallized in the tri-cyclic ethylamine solution, dehydrated with dehydration, got the finished product butyl butyrate.
Figure 1
2018100824 19 Jun 2018
Nitro-cotton intermediates butyl butyrate synthesis method
FIELD OF THE INVENTION
The present invention relates to a method for preparing a pharmaceutical 5 intermediate which belongs to the field of organic synthesis, more particularly, relates to nitro-cotton intermediates butyl butyrate synthesis method.
GENERAL BACKGROUND
Butyl butyrate is mainly applied to nitrocellulose, shellac, coumarone resin and coatings, it can be used as a spice which is mainly used to contain apples, pineapple and other flavors, it can also be used as a chromatographic analysis of standard substances and solvents, but also used for organic synthesis. However, most of the existing synthesis methods are using the method the n-butyl alcohol is heated at 400°C, and finally formed by reaction of manganese dioxide. This method needs a very high temperature environment, and high demand for energy consumption, it has higher requirements on the heat resistance of the equipment and maintenance costs, it is not conducive to reduce the production cost, but also need manganese dioxide as reaction, and manganese dioxide is a kind of serious pollution to the environment, the cost of follow-up pollution treatment is higher, and the synthesis method is complicated.
Therefore, it is necessary to propose a new synthesis method.
SUMMARY
Based on the technical problems of the background technology, the purpose of the present invention is to provide nitro-cotton intermediates butyl butyrate synthesis method, comprises the following steps:
A: 2-amino-butanone, 1.7L potassium chloride solution were added to the reaction vessel, raised the temperature of the solution to 35-42°C, controlled the stirring speed at 230-250 rpm, reacted for 30-50min, added 900ml anisole solution, raised the temperature of the solution to 45-50°C, continued to react for 90-110 min;
B: added benzyl benzoate solution, ruthenium dioxide powder, raised the stirring
2018100824 19 Jun 2018 speed at 3l0-330rpm, continued to react for 60-90min, added 1.3L sodium sulfate solution, set aside for l-2h, stratified solution, separated reservoir, washed with the ethyl cyanide solution for several times, washed with the pyridine solution for several times, re-crystallized in the tri-cyclic ethylamine solution, dehydrated with dehydration, got the finished product butyl butyrate.
Preferably, the potassium chloride solution has a mass fraction of 10-16%.
Preferably, the mass fraction of the anisole solution is 20-25%.
Preferably, the mass fraction of the benzyl benzoate solution is 30-36%.
Preferably, the sodium sulfate solution has a mass fraction of 15-22%.
Preferably, the mass fraction of ethyl cyanide solution is 35-42%.
Preferably, the pyridine solution has a mass fraction of 50-56%.
Preferably, the mass fraction of tri-cyclic ethylamine solution is 70-75%.
Throughout the reaction process can be the following reaction formula:
CU3 h£c^ C.H + C|4H|,O2 + RuO2 -Ch3(Ch2)2COO(Ch2)3Ch3
Compared with the synthetic method disclosed in the background art, the invention provides nitro-cotton intermediates butyl butyrate synthesis method, it is unnecessary to use the method that n-butyl alcohol heated at 40032, and finally formed by reaction of manganese dioxide. It doesn’t need reaction at very high temperatures, and reduces the demand for energy consumption, reduces the requirements on the heat resistance of the equipment and maintenance costs, it is unnecessary to use manganese dioxide as reaction, and reduce manganese dioxide’s pollution to the environment, the cost of follow-up pollution treatment is low, reducing intermediate links reaction, decreasing the reaction Lime and improving the reaction yield, at the same time, the present invention provides a new synthetic route which has offered a good foundation for further enhancing the yield of the reaction.
2018100824 19 Jun 2018
DESCRIPTION OF THE DRAWINGS
Figure 1 is the infrared analysis spectrum of finished product butyl butyrate.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
The following examples with reference to specific embodiments of the present invention are further illustrated:
Embodiment 1
Nitro-cotton intermediates butyl butyrate synthesis method comprises the following steps:
A: 3mol 2-amino-butanone, 1.7L potassium chloride solution with a mass fraction of 10% were added to the reaction vessel, raised the temperature of the solution to 35°C, controlled the stirring speed at 230rpm, reacted for 30min, added 900ml anisole solution with a mass fraction of 20%, raised the temperature of the solution to 45°C, continued to react for 90min;
B: added 6mol benzyl benzoate solution with a mass fraction of 30%, 3mol ruthenium dioxide powder, raised the stirring speed at 310rpm, continued to react for 60min, added 1.3L sodium sulfate solution with a mass fraction of 15%, set aside for lh, stratified solution, separated reservoir, washed with the ethyl cyanide solution with a mass fraction of 35% for two times, washed with the pyridine solution with a mass fraction of 50% for five times, re-crystallized in the tri-cyclic ethylamine solution with a mass fraction of 70%, dehydrated with anhydrous magnesium sulfate dehydration, got the finished product butyl butyrate 380.16g, yield of 88%.
Embodiment 2
Nitro-cotton intermediates butyl butyrate synthesis method comprises the following steps:
A: 3mol 2-amino-butanone, 1.7L potassium chloride solution with a mass fraction of 14% were added to the reaction vessel, raised the temperature of the solution to 38°C, controlled the stirring speed at 240rpm, reacted for 40min, added
900ml anisole solution with a mass fraction of 24%, raised the temperature of the
2018100824 19 Jun 2018 solution to 48°C, continued to react for lOOmin;
B: added 6.8mol benzyl benzoate solution with a mass fraction of 32%, 3.5mol ruthenium dioxide powder, raised the stirring speed at 320rpm, continued to react for 75min, added 1.3L sodium sulfate solution with a mass fraction of 19%, set aside for
1.5h, stratified solution, separated reservoir, washed with the ethyl cyanide solution with a mass fraction of 39% for three times, washed with the pyridine solution with a mass fraction of 55% for six times, re-crystallized in the tri-cyclic ethylamine solution with a mass fraction of 73%, dehydrated with anhydrous magnesium sulfate dehydration, got the finished product butyl butyrate 393.12g, yield of 91%.
Embodiment 3
Nitro-cotton intermediates butyl butyrate synthesis method comprises the following steps:
A: 3mol 2-amino-butanone, 1.7L potassium chloride solution with a mass 15 fraction of 16% were added to the reaction vessel, raised the temperature of the solution to 42°C, controlled the stirring speed at 250rpm, reacted for 50min, added 900ml anisole solution with a mass fraction of 25%, raised the temperature of the solution to 50°C, continued to react for llOmin;
B: added 7mol benzyl benzoate solution with a mass fraction of 36%, 4mol 20 ruthenium dioxide powder, raised the stirring speed at 330rpm, continued to react for 90min, added 1.3L sodium sulfate solution with a mass fraction of 22%, set aside for 2h, stratified solution, separated reservoir, washed with the ethyl cyanide solution with a mass fraction of 42% for four times, washed with the pyridine solution with a mass fraction of 56% for seven times, re-crystallized in the tri-cyclic ethylamine solution with a mass fraction of 75%, dehydrated with anhydrous magnesium sulfate dehydration, got the finished product butyl butyrate 410.4g, yield of 95%.
Infrared analysis of finished product butyl butyrate, infrared spectrum is shown in figure 1, the analysis of data is shown in Table 1:
Table 1 Peak data
2018100824 19 Jun 2018
| Serial | Peak position | Transmittance | Half width | Peak difference |
| number | (cm'1) | (%) | (cnf1) | (%) |
| 1 | 926 | 66 | 38 | 14 |
| 2 | 1002 | 29 | 22 | 53 |
| 3 | 1076 | 22 | 27 | 30 |
| 4 | 1155 | 9 | 69 | 24 |
| 5 | 1194 | 9 | 60 | 23 |
| 6 | 1257 | 30 | 56 | 21 |
| 7 | 1345 | 41 | 42 | 24 |
| 8 | 1386 | 31 | 42 | 36 |
| 9 | 1467 | 19 | 37 | 63 |
| 10 | 1732 | 9 | 56 | 87 |
| 11 | 2972 | 12 | 147 | 83 |
The embodiments of the present invention are merely preferred embodiments of the present invention, but the range of the present invention is not limited this, and any person who is familiar with those skilled in the arts, within the technical range of the present invention. It is intended that the technical solution and its inventive concept be replaced or modified equivalently with reference to the range of the invention.
2018100824 19 Jun 2018
Claims (4)
- Claims1. Nitro-cotton intermediates butyl butyrate synthesis method, comprise the following steps:A:
- 2-amino-butanone, 1.7L potassium chloride solution were added to the reaction vessel, raised the temperature of the solution to 35-42°C, controlled the stirring speed at 230-250 rpm, reacted for 30-50min, added 900ml anisole solution, raised the temperature of the solution to 45-50°C, continued to react for 90-110 min;B: added benzyl benzoate solution, ruthenium dioxide powder, raised the stirring speed at 310-330rpm, continued to react for 60-90min, added 1.3L sodium sulfate solution, set aside for l-2h, stratified solution, separated reservoir, washed with the ethyl cyanide solution for several times, washed with the pyridine solution for several times, re-crystallized in the tri-cyclic ethylamine solution, dehydrated with dehydration, got the finished product butyl butyrate.15 2. Nitro-cotton intermediates butyl butyrate synthesis method according to claim1 wherein the potassium chloride solution has a mass fraction of 10-16%.
- 3. Nitro-cotton intermediates butyl butyrate synthesis method according to claim 1 wherein the mass fraction of the anisole solution is 20-25%.
- 4. Nitro-cotton intermediates butyl butyrate synthesis method according to claim20 1 wherein the mass fraction of the benzyl benzoate solution is 30-36%.2018100824 19 Jun 20181/1Figure 1
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710529201.4A CN108238930A (en) | 2017-07-01 | 2017-07-01 | The synthetic method of nitrocellulose intermediate butyl butyrate |
| CN2017105292014 | 2017-07-01 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| AU2018100824A4 true AU2018100824A4 (en) | 2018-08-02 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| AU2018100824A Ceased AU2018100824A4 (en) | 2017-07-01 | 2018-06-19 | Nitro-cotton intermediates butyl butyrate synthesis method |
Country Status (4)
| Country | Link |
|---|---|
| CN (1) | CN108238930A (en) |
| AU (1) | AU2018100824A4 (en) |
| GB (1) | GB201713403D0 (en) |
| IE (1) | IES87002B2 (en) |
-
2017
- 2017-07-01 CN CN201710529201.4A patent/CN108238930A/en active Pending
- 2017-08-21 GB GBGB1713403.2A patent/GB201713403D0/en not_active Ceased
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2018
- 2018-06-19 AU AU2018100824A patent/AU2018100824A4/en not_active Ceased
- 2018-06-26 IE IES20180190A patent/IES87002B2/en unknown
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| Publication number | Publication date |
|---|---|
| IES20180190A2 (en) | 2019-05-01 |
| CN108238930A (en) | 2018-07-03 |
| IES87002B2 (en) | 2019-05-01 |
| GB201713403D0 (en) | 2017-10-04 |
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