CN109836447A - A kind of preparation method of double trimethyl silicon substrate potassamides - Google Patents
A kind of preparation method of double trimethyl silicon substrate potassamides Download PDFInfo
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- CN109836447A CN109836447A CN201711198200.2A CN201711198200A CN109836447A CN 109836447 A CN109836447 A CN 109836447A CN 201711198200 A CN201711198200 A CN 201711198200A CN 109836447 A CN109836447 A CN 109836447A
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- preparation
- potassamides
- silicon substrate
- metallic potassium
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Abstract
The invention belongs to chemical intermediate preparation fields, and in particular to a kind of preparation method of double trimethyl silicon substrate potassamides.Therefore the characteristics of present invention preparation method method includes 5 steps, has high income, and raw material is cheap, and process is simple, good product quality has certain application value.
Description
Technical field
The invention belongs to chemical intermediate preparation fields, and in particular to a kind of preparation side of double trimethyl silicon substrate potassamides
Method.
Background technique
Double trimethyl silicon substrate potassamide Potassium bis (trimethylsilyl) amide, abbreviation KHMDS are a kind of
Big steric hindrance organic alkali, and other big steric hindrance organic alkalis, such as lithium diisopropylamine, double trimethyl silicon substrate lithium amides, double three
Methylsilyl Sodamide etc. is compared, and effect is similar, but alkalinity is stronger, has its unique place in certain reactions, there is other
The advantage that organic base does not have.
But double trimethyl silicon substrate potassamides are currently without preferable preparation method, the useful hydrofining of classical way and pregnancy
The reaction of base disilazane, hydrofining is expensive, limits a large amount of uses of this method, and generate hydrogen in reaction, exists
Certain security risk.Hydrofining is also to prepare from metallic potassium, if can directly be prepared with metallic potassium, can undoubtedly be dropped
Low production cost, the bigger production scale and application range for expanding the reagent.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation method of double trimethyl silicon substrate potassamides, this method high income is closed
At simple, suitable industrialized production.
To achieve the goals above, the present invention adopts the following technical scheme:
A kind of preparation method of double trimethyl silicon substrate potassamides, which is characterized in that the preparation method method includes the following steps:
Step 1: constant pressure funnel will be housed, the clean reaction kettle inert gas replacement of reflux condensing tube three times, is added and weighs
Accurate hexamethyldisilazane and atent solvent；
Step 2: using atent solvent, such as alkanes, aromatic hydrocarbon solvent washes away the paraffin oil of metallic potassium package, removes outside metallic potassium
Layer oxide, and by bright as new metallic potassium is placed in the reaction solution of step 1；
Step 3: opening stirring, heating, the reaction mixture that step 2 is obtained is warming up to 90 degree, and metallic potassium is molten in 63 degree of beginnings
Solution, forms fine drop under stirring；
Step 4: the isoprene or styrene of accurate measurement is slowly added dropwise, heats up during being added dropwise obvious, speed is added dropwise in control
Degree maintains 90-120 DEG C of reacting liquid temperature, during dropwise addition, if reaction system becomes viscous, continuously adds toluene in batches, just
The high boiling inert solvent such as heptane promotes stirring smooth；
Step 5: after being added dropwise, continuing stirring and all disappear to metallic potassium, then it is molten that a large amount of alkane badness are added in cooling
Agent continues stirring to room temperature, obtains the suspension of KHMDS, anhydrous and oxygen-free filtering can obtain KHMDS sterling, can configure as needed
The solution of various specifications, or directly with sterling packing and selling.
A kind of preparation method of double trimethyl silicon substrate potassamides, which is characterized in that atent solvent in the preparation method step 1
For toluene, ethylbenzene, normal heptane, tetrahydrofuran etc..
A kind of preparation method of double trimethyl silicon substrate potassamides, which is characterized in that reaction temperature in the preparation method step 3
It is 100-110 DEG C.
Compared with prior art, effect of the invention is that: this preparation method have high income, raw material is cheap, at technique
Therefore the characteristics of reason is simple, good product quality has certain application value.
Specific embodiment
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, made any to repair
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Embodiment 1
A kind of preparation method of double trimethyl silicon substrate potassamides, which is characterized in that the preparation method method includes the following steps:
Step 1: constant pressure funnel will be housed, the clean reaction kettle inert gas replacement of reflux condensing tube three times, is added and weighs
Accurate hexamethyldisilazane and toluene；
Step 2: using atent solvent, such as alkanes, aromatic hydrocarbon solvent washes away the paraffin oil of metallic potassium package, removes outside metallic potassium
Layer oxide, and by bright as new metallic potassium is placed in the reaction solution of step 1；
Step 3: opening stirring, heating, the reaction mixture that step 2 is obtained is warming up to 90 degree, and metallic potassium is molten in 63 degree of beginnings
Solution, forms fine drop under stirring；
Step 4: the isoprene or styrene of accurate measurement is slowly added dropwise, heats up during being added dropwise obvious, speed is added dropwise in control
Degree maintains 90-120 DEG C of reacting liquid temperature, during dropwise addition, if reaction system becomes viscous, continuously adds toluene in batches, just
The high boiling inert solvent such as heptane promotes stirring smooth；
Step 5: after being added dropwise, continuing stirring and all disappear to metallic potassium, then it is molten that a large amount of alkane badness are added in cooling
Agent continues stirring to room temperature, obtains the suspension of KHMDS, anhydrous and oxygen-free filtering can obtain KHMDS sterling, can configure as needed
The solution of various specifications, or directly with sterling packing and selling.
Embodiment 2
A kind of preparation method of double trimethyl silicon substrate potassamides, which is characterized in that the preparation method method includes the following steps:
Step 1: constant pressure funnel will be housed, the clean reaction kettle inert gas replacement of reflux condensing tube three times, is added and weighs
Accurate hexamethyldisilazane and ethylbenzene；
Step 2: using atent solvent, such as alkanes, aromatic hydrocarbon solvent washes away the paraffin oil of metallic potassium package, removes outside metallic potassium
Layer oxide, and by bright as new metallic potassium is placed in the reaction solution of step 1；
Step 3: opening stirring, heating, the reaction mixture that step 2 is obtained is warming up to 90 degree, and metallic potassium is molten in 63 degree of beginnings
Solution, forms fine drop under stirring；
Step 4: the isoprene or styrene of accurate measurement is slowly added dropwise, heats up during being added dropwise obvious, speed is added dropwise in control
Degree maintains 90-120 DEG C of reacting liquid temperature, during dropwise addition, if reaction system becomes viscous, continuously adds toluene in batches, just
The high boiling inert solvent such as heptane promotes stirring smooth；
Step 5: after being added dropwise, continuing stirring and all disappear to metallic potassium, then it is molten that a large amount of alkane badness are added in cooling
Agent continues stirring to room temperature, obtains the suspension of KHMDS, anhydrous and oxygen-free filtering can obtain KHMDS sterling, can configure as needed
The solution of various specifications, or directly with sterling packing and selling.
Embodiment 3
A kind of preparation method of double trimethyl silicon substrate potassamides, which is characterized in that the preparation method method includes the following steps:
Step 1: constant pressure funnel will be housed, the clean reaction kettle inert gas replacement of reflux condensing tube three times, is added and weighs
Accurate hexamethyldisilazane and tetrahydrofuran；
Step 2: using atent solvent, such as alkanes, aromatic hydrocarbon solvent washes away the paraffin oil of metallic potassium package, removes outside metallic potassium
Layer oxide, and by bright as new metallic potassium is placed in the reaction solution of step 1；
Step 3: opening stirring, heating, the reaction mixture that step 2 is obtained is warming up to 90 degree, and metallic potassium is molten in 63 degree of beginnings
Solution, forms fine drop under stirring；
Step 4: the isoprene or styrene of accurate measurement is slowly added dropwise, heats up during being added dropwise obvious, speed is added dropwise in control
Degree maintains 90-120 DEG C of reacting liquid temperature, during dropwise addition, if reaction system becomes viscous, continuously adds toluene in batches, just
The high boiling inert solvent such as heptane promotes stirring smooth；
Step 5: after being added dropwise, continuing stirring and all disappear to metallic potassium, then it is molten that a large amount of alkane badness are added in cooling
Agent continues stirring to room temperature, obtains the suspension of KHMDS, anhydrous and oxygen-free filtering can obtain KHMDS sterling, can configure as needed
The solution of various specifications, or directly with sterling packing and selling.
Claims (3)
1. a kind of preparation method of double trimethyl silicon substrate potassamides, which is characterized in that the preparation method method includes the following steps:
Step 1: constant pressure funnel will be housed, the clean reaction kettle inert gas replacement of reflux condensing tube three times, is added and weighs
Accurate hexamethyldisilazane and atent solvent；
Step 2: using atent solvent, such as alkanes, aromatic hydrocarbon solvent washes away the paraffin oil of metallic potassium package, removes outside metallic potassium
Layer oxide, and by bright as new metallic potassium is placed in the reaction solution of step 1；
Step 3: opening stirring, heating, the reaction mixture that step 2 is obtained is warming up to 90 degree, and metallic potassium is molten in 63 degree of beginnings
Solution, forms fine drop under stirring；
Step 4: the isoprene or styrene of accurate measurement is slowly added dropwise, heats up during being added dropwise obvious, speed is added dropwise in control
Degree maintains 90-120 DEG C of reacting liquid temperature, during dropwise addition, if reaction system becomes viscous, continuously adds toluene in batches, just
The high boiling inert solvent such as heptane promotes stirring smooth；
Step 5: after being added dropwise, continuing stirring and all disappear to metallic potassium, then it is molten that a large amount of alkane badness are added in cooling
Agent continues stirring to room temperature, obtains the suspension of KHMDS, anhydrous and oxygen-free filtering can obtain KHMDS sterling, can configure as needed
The solution of various specifications, or directly with sterling packing and selling.
2. a kind of preparation method of double trimethyl silicon substrate potassamides according to claim 1, which is characterized in that the preparation side
Atent solvent is toluene, ethylbenzene, normal heptane, tetrahydrofuran etc. in method step 1.
3. a kind of preparation method of double trimethyl silicon substrate potassamides according to claim 1, which is characterized in that the preparation side
Reaction temperature is 100-110 DEG C in method step 3.
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| CN201711198200.2A CN109836447A (en) | 2017-11-25 | 2017-11-25 | A kind of preparation method of double trimethyl silicon substrate potassamides |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112707929A (en) * | 2020-12-24 | 2021-04-27 | 绍兴上虞华伦化工有限公司 | Process for preparing bis (trimethyl disilyl) lithium amide |
-
2017
- 2017-11-25 CN CN201711198200.2A patent/CN109836447A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112707929A (en) * | 2020-12-24 | 2021-04-27 | 绍兴上虞华伦化工有限公司 | Process for preparing bis (trimethyl disilyl) lithium amide |
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Application publication date: 20190604 |