CN108203397A - A kind of synthetic method of organic synthesis intermediate acetoxime - Google Patents
A kind of synthetic method of organic synthesis intermediate acetoxime Download PDFInfo
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- CN108203397A CN108203397A CN201611171023.4A CN201611171023A CN108203397A CN 108203397 A CN108203397 A CN 108203397A CN 201611171023 A CN201611171023 A CN 201611171023A CN 108203397 A CN108203397 A CN 108203397A
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- acetoxime
- organic synthesis
- synthetic method
- synthesis intermediate
- solution temperature
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C249/00—Preparation of compounds containing nitrogen atoms doubly-bound to a carbon skeleton
- C07C249/04—Preparation of compounds containing nitrogen atoms doubly-bound to a carbon skeleton of oximes
- C07C249/08—Preparation of compounds containing nitrogen atoms doubly-bound to a carbon skeleton of oximes by reaction of hydroxylamines with carbonyl compounds
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
A kind of synthetic method of organic synthesis intermediate acetoxime, mainly includes the following steps：The phosphatic hydroxylamine of 0.5mol is dissolved in 20L Klorvess Liquids, it is slowly added to 0.6-0.8mol acetone solns, it is 35 39 DEG C to control solution temperature, 90-110min is stood after adding, solution temperature is reduced to 31-34 DEG C, it is 8.5-9 to add in 0.9mol potassium bicarbonate solutions and adjust solution ph, and control solution temperature is 41-45 DEG C, is layered after cooling, detach oil-yielding stratum, 90-95 DEG C of fraction, cyclohexane solution washing are collected in vacuum distillation, aqueous isopropanol washs, dehydrating agent is dehydrated, and crystallisation by cooling obtains finished product acetoxime.
Description
Technical field
The present invention relates to a kind of synthetic methods of organic synthesis intermediate acetoxime.
Background technology
Acetoxime is mainly used for organic synthesis intermediate, can be used for the qualification process of the metal ions such as nickel, cobalt, water
Solution is in neutrality, and potassium permanganate can be made to fade at normal temperatures, is mainly used for feedwater chemistry oxygen scavenger in Industrial Boiler, with tradition
Boiler chemical oxygen scavenger is compared, and is had the characteristics of dosage is few, and oxygen removal efficiency is high, nontoxic, nonpollution environment, is stopping for boilers
With protection and the best drug of Passivation Treatment, still, existing synthetic method makees reactant, process ratio using sodium hydroxide mostly
More complicated, ultimate yield is simultaneously not bery high, therefore, it is necessary to propose a kind of new synthetic method, this is for further improving product
Quality and yield, reduce by-products content have important economic implications.
Invention content
The purpose of the present invention is to provide a kind of synthetic methods of organic synthesis intermediate acetoxime, include the following steps：
(i) phosphatic hydroxylamine of 0.5mol is dissolved in 20L Klorvess Liquids, is slowly added to 0.6-0.8mol acetone solns,
It is 35--39 DEG C to control solution temperature, and 90-110min is stood after adding, and reduces solution temperature to 31-34 DEG C, adds in 0.9mol
It is 8.5-9 that potassium bicarbonate solution, which adjusts solution ph, and control solution temperature is 41-45 DEG C, is layered after cooling, and separation is fuel-displaced
Layer, vacuum distillation, the fraction of 90-95 DEG C of collection, cyclohexane solution washing, aqueous isopropanol washing, dehydrating agent dehydration, cooling
Crystallization, obtains finished product acetoxime；Wherein, the Klorvess Liquid mass fraction described in step (i) is 15-20%, and step (i) is described
Acetone soln mass fraction for 30-35%, the potassium bicarbonate solution mass fraction described in step (i) is 20-25%, step
(i) pressure residing for the vacuum distillation described in is 50-55kPa, cyclohexane solution mass fraction described in step (i) for 70-
75%, the aqueous isopropanol mass fraction described in step (i) is 90-96%, and the dehydrating agent described in step (i) is Carbon Dioxide
Any one in potassium, dead plaster.
Entire reaction process can be represented with following reaction formula：
The invention has the advantages that：Reduce the intermediate link of reaction, shorten the reaction time, improve reaction yield.
Specific embodiment
With reference to specific implementation example, the invention will be further described：
A kind of synthetic method of organic synthesis intermediate acetoxime,
Example 1：
The phosphatic hydroxylamine of 0.5mol is dissolved in 20L mass fractions as 15% Klorvess Liquid, is slowly added to 0.6mol matter
Amount score is 30% acetone soln, and control solution temperature is 35 DEG C, and 90min is stood after adding, and reduces solution temperature to 31 DEG C, adds
Enter 0.9mol mass fractions be 20% potassium bicarbonate solution adjust solution ph be 8.5, control solution temperature be 41 DEG C, after cooling
Layering detaches oil-yielding stratum, and 50kPa vacuum distillations, the fraction of 90 DEG C of collection, mass fraction is that 70% cyclohexane solution washs, matter
Score to be measured to wash for 90% aqueous isopropanol, Anhydrous potassium carbonate dehydrating agent dehydration, crystallisation by cooling obtains finished product acetoxime 33.215g,
Yield 91%.
Example 2：
The phosphatic hydroxylamine of 0.5mol is dissolved in 20L mass fractions as 17% Klorvess Liquid, is slowly added to 0.7mol matter
Amount score is 32% acetone soln, and control solution temperature is 37 DEG C, and 100min is stood after adding, and reduces solution temperature to 32 DEG C,
Addition 0.9mol mass fractions are that 22% potassium bicarbonate solution adjusting solution ph is 8.7, and control solution temperature is 43 DEG C, cooling
After be layered, detach oil-yielding stratum, 93 DEG C of fraction is collected in 53kPa vacuum distillations, and mass fraction is the washing of 72% cyclohexane solution,
Mass fraction is washed for 93% aqueous isopropanol, and dead plaster dehydrating agent dehydration, crystallisation by cooling obtains finished product acetoxime
33.945g yield 93%.
Example 3：
The phosphatic hydroxylamine of 0.5mol is dissolved in 20L mass fractions as 20% Klorvess Liquid, is slowly added to 0.8mol matter
Amount score is 35% acetone soln, and control solution temperature is 39 DEG C, and 110min is stood after adding, and reduces solution temperature to 34 DEG C,
Addition 0.9mol mass fractions are that 25% potassium bicarbonate solution adjusting solution ph is 9, and control solution temperature is 45 DEG C, after cooling
Layering detaches oil-yielding stratum, and 55kPa vacuum distillations, the fraction of 95 DEG C of collection, mass fraction is that 75% cyclohexane solution washs, matter
Score to be measured to wash for 96% aqueous isopropanol, Anhydrous potassium carbonate dehydrating agent dehydration, crystallisation by cooling obtains finished product acetoxime 35.04g,
Yield 96%.
Claims (4)
1. a kind of synthetic method of organic synthesis intermediate acetoxime, which is characterized in that mainly include the following steps：(i) will
The phosphatic hydroxylamine of 0.5mol is dissolved in 20L Klorvess Liquids, is slowly added to 0.6-0.8mol acetone solns, controls solution temperature
It is 35--39 DEG C, 90-110min is stood after adding, reduces solution temperature to 31-34 DEG C, add in 0.9mol potassium bicarbonate solutions
It is 8.5-9 to adjust solution ph, and control solution temperature is 41-45 DEG C, is layered after cooling, detaches oil-yielding stratum, is evaporated under reduced pressure, and is received
The fraction of 90-95 DEG C of collection, cyclohexane solution washing, aqueous isopropanol washing, dehydrating agent dehydration, crystallisation by cooling obtain finished product acetone
Oxime；Wherein, the Klorvess Liquid mass fraction described in step (i) is 15-20%, the acetone soln quality point described in step (i)
Number is 30-35%, and the potassium bicarbonate solution mass fraction described in step (i) is 20-25%, and the decompression described in step (i) is steamed
It is 50-55kPa to evaporate residing pressure.
A kind of 2. synthetic method of organic synthesis intermediate acetoxime according to claim 1, which is characterized in that step (i)
The cyclohexane solution mass fraction is 70-75%.
A kind of 3. synthetic method of organic synthesis intermediate acetoxime according to claim 1, which is characterized in that step (i)
The aqueous isopropanol mass fraction is 90-96%.
A kind of 4. synthetic method of organic synthesis intermediate acetoxime according to claim 1, which is characterized in that step (i)
The dehydrating agent is any one in Anhydrous potassium carbonate, dead plaster.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611171023.4A CN108203397A (en) | 2016-12-16 | 2016-12-16 | A kind of synthetic method of organic synthesis intermediate acetoxime |
| GBGB1700008.4A GB201700008D0 (en) | 2016-12-16 | 2017-01-02 | Organic synthesis intermediates aceton oxime synthesis method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611171023.4A CN108203397A (en) | 2016-12-16 | 2016-12-16 | A kind of synthetic method of organic synthesis intermediate acetoxime |
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| Publication Number | Publication Date |
|---|---|
| CN108203397A true CN108203397A (en) | 2018-06-26 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201611171023.4A Pending CN108203397A (en) | 2016-12-16 | 2016-12-16 | A kind of synthetic method of organic synthesis intermediate acetoxime |
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| CN (1) | CN108203397A (en) |
| GB (1) | GB201700008D0 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112679379A (en) * | 2020-12-23 | 2021-04-20 | 浙江锦华新材料股份有限公司 | Preparation method of acetoxime |
-
2016
- 2016-12-16 CN CN201611171023.4A patent/CN108203397A/en active Pending
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2017
- 2017-01-02 GB GBGB1700008.4A patent/GB201700008D0/en not_active Ceased
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112679379A (en) * | 2020-12-23 | 2021-04-20 | 浙江锦华新材料股份有限公司 | Preparation method of acetoxime |
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| GB201700008D0 (en) | 2017-02-15 |
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Application publication date: 20180626 |