CN108503668A - A kind of synthetic method of trimethyl phenoxysilane - Google Patents
A kind of synthetic method of trimethyl phenoxysilane Download PDFInfo
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- OJAJJFGMKAZGRZ-UHFFFAOYSA-N trimethyl(phenoxy)silane Chemical compound C[Si](C)(C)OC1=CC=CC=C1 OJAJJFGMKAZGRZ-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 238000010189 synthetic method Methods 0.000 title claims abstract description 17
- 238000006243 chemical reaction Methods 0.000 claims abstract description 41
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 claims abstract description 27
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000003054 catalyst Substances 0.000 claims abstract description 19
- 239000002994 raw material Substances 0.000 claims abstract description 10
- VHYFNPMBLIVWCW-UHFFFAOYSA-N 4-Dimethylaminopyridine Chemical compound CN(C)C1=CC=NC=C1 VHYFNPMBLIVWCW-UHFFFAOYSA-N 0.000 claims description 44
- FYGHSUNMUKGBRK-UHFFFAOYSA-N 1,2,3-trimethylbenzene Chemical compound CC1=CC=CC(C)=C1C FYGHSUNMUKGBRK-UHFFFAOYSA-N 0.000 claims description 4
- 230000008719 thickening Effects 0.000 claims description 2
- 229940125904 compound 1 Drugs 0.000 abstract description 18
- 150000001875 compounds Chemical class 0.000 abstract description 11
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 238000000034 method Methods 0.000 abstract description 8
- -1 that is Chemical compound 0.000 abstract description 5
- DXRFZHILMCWCNG-UHFFFAOYSA-N N,N-dimethyl-1,8-naphthyridin-2-amine Chemical class C1=CC=NC2=NC(N(C)C)=CC=C21 DXRFZHILMCWCNG-UHFFFAOYSA-N 0.000 abstract 3
- 239000012141 concentrate Substances 0.000 abstract 1
- 239000007788 liquid Substances 0.000 abstract 1
- AICOOMRHRUFYCM-ZRRPKQBOSA-N oxazine, 1 Chemical compound C([C@@H]1[C@H](C(C[C@]2(C)[C@@H]([C@H](C)N(C)C)[C@H](O)C[C@]21C)=O)CC1=CC2)C[C@H]1[C@@]1(C)[C@H]2N=C(C(C)C)OC1 AICOOMRHRUFYCM-ZRRPKQBOSA-N 0.000 abstract 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 12
- 229960000549 4-dimethylaminophenol Drugs 0.000 description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 8
- 230000015572 biosynthetic process Effects 0.000 description 7
- 239000007858 starting material Substances 0.000 description 7
- 238000003786 synthesis reaction Methods 0.000 description 7
- 229910021529 ammonia Inorganic materials 0.000 description 6
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 description 6
- 238000009413 insulation Methods 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 239000002253 acid Substances 0.000 description 5
- 238000006561 solvent free reaction Methods 0.000 description 5
- 230000006837 decompression Effects 0.000 description 4
- 239000000377 silicon dioxide Substances 0.000 description 4
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 3
- 229940125782 compound 2 Drugs 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 231100000419 toxicity Toxicity 0.000 description 3
- 230000001988 toxicity Effects 0.000 description 3
- 239000002351 wastewater Substances 0.000 description 3
- 235000010894 Artemisia argyi Nutrition 0.000 description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 2
- HEDRZPFGACZZDS-MICDWDOJSA-N Trichloro(2H)methane Chemical compound [2H]C(Cl)(Cl)Cl HEDRZPFGACZZDS-MICDWDOJSA-N 0.000 description 2
- 244000030166 artemisia Species 0.000 description 2
- AXZHOFSSTJKWJE-UHFFFAOYSA-N bismuth;trifluoromethanesulfonic acid Chemical compound [Bi].OS(=O)(=O)C(F)(F)F AXZHOFSSTJKWJE-UHFFFAOYSA-N 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 229910052681 coesite Inorganic materials 0.000 description 2
- 229910052906 cristobalite Inorganic materials 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910000077 silane Inorganic materials 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- WBHQBSYUUJJSRZ-UHFFFAOYSA-M sodium bisulfate Chemical compound [Na+].OS([O-])(=O)=O WBHQBSYUUJJSRZ-UHFFFAOYSA-M 0.000 description 2
- 229910000342 sodium bisulfate Inorganic materials 0.000 description 2
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 229910052682 stishovite Inorganic materials 0.000 description 2
- 229960004556 tenofovir Drugs 0.000 description 2
- LDEKQSIMHVQZJK-CAQYMETFSA-N tenofovir alafenamide Chemical compound O([P@@](=O)(CO[C@H](C)CN1C2=NC=NC(N)=C2N=C1)N[C@@H](C)C(=O)OC(C)C)C1=CC=CC=C1 LDEKQSIMHVQZJK-CAQYMETFSA-N 0.000 description 2
- 229960004946 tenofovir alafenamide Drugs 0.000 description 2
- SVUJNSGGPUCLQZ-FQQAACOVSA-N tenofovir alafenamide fumarate Chemical compound OC(=O)\C=C\C(O)=O.O([P@@](=O)(CO[C@H](C)CN1C2=NC=NC(N)=C2N=C1)N[C@@H](C)C(=O)OC(C)C)C1=CC=CC=C1.O([P@@](=O)(CO[C@H](C)CN1C2=NC=NC(N)=C2N=C1)N[C@@H](C)C(=O)OC(C)C)C1=CC=CC=C1 SVUJNSGGPUCLQZ-FQQAACOVSA-N 0.000 description 2
- VCMJCVGFSROFHV-WZGZYPNHSA-N tenofovir disoproxil fumarate Chemical compound OC(=O)\C=C\C(O)=O.N1=CN=C2N(C[C@@H](C)OCP(=O)(OCOC(=O)OC(C)C)OCOC(=O)OC(C)C)C=NC2=C1N VCMJCVGFSROFHV-WZGZYPNHSA-N 0.000 description 2
- 229910052905 tridymite Inorganic materials 0.000 description 2
- 238000005160 1H NMR spectroscopy Methods 0.000 description 1
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 description 1
- TZRXHJWUDPFEEY-UHFFFAOYSA-N Pentaerythritol Tetranitrate Chemical compound [O-][N+](=O)OCC(CO[N+]([O-])=O)(CO[N+]([O-])=O)CO[N+]([O-])=O TZRXHJWUDPFEEY-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 241000218636 Thuja Species 0.000 description 1
- UMVBXBACMIOFDO-UHFFFAOYSA-N [N].[Si] Chemical compound [N].[Si] UMVBXBACMIOFDO-UHFFFAOYSA-N 0.000 description 1
- PEEJXKHXJXFVIA-UHFFFAOYSA-N [O].CC=1C(=C(C=CC1)C)C Chemical compound [O].CC=1C(=C(C=CC1)C)C PEEJXKHXJXFVIA-UHFFFAOYSA-N 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 150000001540 azides Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000001684 chronic effect Effects 0.000 description 1
- 230000001447 compensatory effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- VFNGKCDDZUSWLR-UHFFFAOYSA-L disulfate(2-) Chemical compound [O-]S(=O)(=O)OS([O-])(=O)=O VFNGKCDDZUSWLR-UHFFFAOYSA-L 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- GEMITLJMEMBDKW-UHFFFAOYSA-N hydrogen sulfate;1h-imidazol-3-ium Chemical compound C1=CNC=N1.OS(O)(=O)=O GEMITLJMEMBDKW-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-M hydrogensulfate Chemical compound OS([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-M 0.000 description 1
- 208000015181 infectious disease Diseases 0.000 description 1
- 208000019423 liver disease Diseases 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 125000002524 organometallic group Chemical group 0.000 description 1
- 125000001820 oxy group Chemical group [*:1]O[*:2] 0.000 description 1
- 125000000951 phenoxy group Chemical group [H]C1=C([H])C([H])=C(O*)C([H])=C1[H] 0.000 description 1
- 239000003419 rna directed dna polymerase inhibitor Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- JRMUNVKIHCOMHV-UHFFFAOYSA-M tetrabutylammonium bromide Chemical compound [Br-].CCCC[N+](CCCC)(CCCC)CCCC JRMUNVKIHCOMHV-UHFFFAOYSA-M 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- ILWRPSCZWQJDMK-UHFFFAOYSA-N triethylazanium;chloride Chemical compound Cl.CCN(CC)CC ILWRPSCZWQJDMK-UHFFFAOYSA-N 0.000 description 1
- PQDJYEQOELDLCP-UHFFFAOYSA-N trimethylsilane Chemical compound C[SiH](C)C PQDJYEQOELDLCP-UHFFFAOYSA-N 0.000 description 1
- 229940094989 trimethylsilane Drugs 0.000 description 1
- SEDZOYHHAIAQIW-UHFFFAOYSA-N trimethylsilyl azide Chemical compound C[Si](C)(C)N=[N+]=[N-] SEDZOYHHAIAQIW-UHFFFAOYSA-N 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/18—Compounds having one or more C—Si linkages as well as one or more C—O—Si linkages
- C07F7/1804—Compounds having Si-O-C linkages
- C07F7/1872—Preparation; Treatments not provided for in C07F7/20
- C07F7/188—Preparation; Treatments not provided for in C07F7/20 by reactions involving the formation of Si-O linkages
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
Abstract
The invention discloses a kind of synthetic methods of trimethyl phenoxysilane, that is, compound 1.Compound 1 is using phenol, hexa methyl silazane as raw material, under the catalyst of 4 dimethylamino naphthyridines, is condensed through a step.Building-up process includes the following steps：（1）, using phenol and hexamethyldisilazane as raw material, 4 dimethylamino naphthyridines make catalyst reaction generate 1 reaction solution of compound；（2）, after reaction, concentrate above-mentioned liquid and obtain 1 finished product of compound.Initiative catalyst of making 4 dimethylamino naphthyridines of the invention is reacted for this step, obtained 1 purity of compound is more than 98%, yield reaches 95% or more, this reaction also has easy to operate, raw material and catalyst is easy to get, production cost is relatively low, is suitble to industrialized production, advantages of environment protection.
Description
Technical field
The present invention relates to pharmaceutical chemistry technical field, specifically a kind of synthetic method of trimethyl phenoxysilane.
Background technology
Tenofovir Chinese mugwort draws phenol amine (tenofovir alafenamide, TAF)（Compound 2）, it is a kind of novel core
Thuja acid reverse transcriptase inhibitor is developed by lucky Leadd B.V, treats chronic HBV infection and compensatory hepatopathy, market
It has good prospects.
Trimethylbenzene oxygroup silicon（Compound 1）For synthesis tenofovir Chinese mugwort draw phenol amine (tenofovir alafenamide,
TAF)（Compound 2）Important source material, dosage is larger.It has been reported that synthetic method listed below.
Method one：
Document（Journal of the Chinese Chemical Society. 2014,61, 929-934.）Report with
Phenol, trim,ethylchlorosilane are raw material, and triethylamine makees acid binding agent, nanoscale niter cake silica（NaHSO4·SiO2）
Make catalyst, trimethyl phenoxysilane is synthesized in acetonitrile or solvent-free reaction（Compound 1）.
The catalyst nano grade niter cake silica that the synthetic method uses（NaHSO4.SiO2）In the market can not
It buys, starting material trim,ethylchlorosilane price is relatively expensive, and the triethylamine hydrochloride of generation generates greatly in last handling process
Measure waste water.
Method two：
Document（Journal of Organic Chemistry. 2001,66, 6734-6737.）It reports with phenol, nitrine
Base trimethyl silane is raw material, and tetrabutylammonium bromide makees catalyst, and solvent-free reaction synthesizes trimethyl phenoxysilane（Compound
1）.
The starting material azidotrimethylsilane that the synthetic method uses is expensive, and cost of material is high, and Azide
Object is explosive.
Method three：
Document（Journal of Organic Chemistry. 1986,51, 3545-3548.）It reports with phenol, front three
Base silicon nitrile is starting material, and solvent-free reaction synthesizes trimethyl phenoxysilane（Compound 1）.
The starting material trimethyl silicane nitrile that the synthetic method uses is expensive, and the cyanide toxicity for reacting generation is very big.
Method four：
Document（Journal of Molecular Catalysis A:Chemical. 2012,365, 15-23.）It reports
Using phenol, hexamethyldisilazane as starting material, 1,3- disulfonic acid imidazole bisulfate（[Dsim]HSO4）Make catalyst, nothing
Solvent reaction synthesizes trimethyl phenoxysilane（Compound 1）；Document（Journal of Molecular Catalysis A:
Chemical. 2011, 349, 63-70.）It reports using phenol, hexamethyldisilazane as starting material, 3- methyl-1s-sulphur
Imidazole acid disulfate makees catalyst, and solvent-free reaction synthesizes trimethyl phenoxysilane（Compound 1）；Document（Journal
of Organometallic Chemistry. 2009, 694, 2562-2566.）It reports with phenol, two silicon nitrogen of hexamethyl
Alkane is starting material, and trifluoromethane sulfonic acid bismuth makees catalyst, and solvent-free reaction synthesizes trimethyl phenoxysilane（Compound 1）.
Catalyst described in above-mentioned document：1,3- disulfonic acid imidazole bisulfate, 3- methyl-1s-sulfonic acid imidazoles hydrogen sulfate
Salt, trifluoromethane sulfonic acid bismuth can not all be bought in the market, be difficult to realize amplification production.
Therefore, it is cheap to find a kind of raw material, catalyst is easily bought in the market, easy to operate, and three waste discharge is few, and yield is higher
Trimethyl phenoxysilane（Compound 1）Synthetic method be necessary.
Invention content
It is an object of the invention to be difficult to buy to solve the existing catalyst for preparing trimethyl phenoxysilane, price
Costliness is more toxic, the unsafe defect of production process and provide a kind of synthetic method of trimethyl phenoxysilane, synthesize
Process includes the following steps：
（1）, with phenol and hexamethyldisilazane（Compound 2）For raw material, with 4-dimethylaminopyridine（DMAP）For catalyst
Reaction generates trimethyl phenoxysilane（Compound 1）Reaction solution；
（2）, after reaction, concentration of reaction solution to 2 inventory mass ratio 1.65 ~ 1.75 of compound obtains 1 trimethyl of compound
Phenoxy group silane finished product.
Reaction principle schematic diagram of the present invention is as follows：
Preferably, step（1）In, reaction temperature is：- 20 ~ 180 ℃.
Preferably, step（1）In, the phenol and the hexamethyldisilazane mass ratio that use are：1 : 1 ~ 1 :
5。
Preferably, step（1）In, phenol and 4-dimethylaminopyridine（DMAP）Mass ratio is：1 : 0.0001 ~
1 : 1。
Preferably, thickening temperature is：20 ~ 150 ℃.
Preferably, step（2）In, concentration pressure is：- 0.1 ~0 MPa.
The beneficial effects of the invention are as follows：It is of the invention initiative by 4-dimethylaminopyridine（DMAP）Make catalyst for this
Step reaction, obtained trimethyl phenoxysilane（Compound 1）Purity is more than 98%, and yield reaches 95% or more, conjunction of the invention
Also there is simple step, raw material at method and catalyst is easy to get, production cost is relatively low, toxicity is low, be suitble to industrialized production, waste water
It is few, advantages of environment protection.
Specific implementation mode
Below in conjunction with specific embodiment, the present invention is further explained：
Raw material used in the present invention is commercially available.
Embodiment 1：The synthesis of compound 1
10.0 g of phenol, 8.6 g of hexamethyldisilazane, 4-dimethylaminopyridine are added into reaction bulb（DMAP）0.1 g is opened
Open stirring, 100 ~ 110 DEG C of temperature control, the ammonia generated with cold water absorbing reaction, after 2 h of insulation reaction, reaction terminates, temperature control
20 ~ 30 DEG C of -0.09 ~ -0.1 MPa of decompression are concentrated to give about 17.2 g of 1 finished product of compound.Yield 97.3%, purity
98.5%。ESI: m/z: 167 [M+H]+. 1H NMR（400 MHz, CDCl3）: δ 7.29-7.25（M, 2H）, 6.97（T,
1H,J= 7.6 Hz）, 6.90（D, 2H,J= 8.0 Hz）, 0.34（S, 9H）.
Embodiment 2：The synthesis of compound 1
10.0 g of phenol, 42.9 g of hexamethyldisilazane, 4-dimethylaminopyridine are added into reaction bulb（DMAP）5.0 g are opened
Open stirring, temperature control -20 ~ -10 DEG C, the ammonia generated with cold water absorbing reaction, after 12 h of insulation reaction, reaction terminates, control
80 ~ 90 DEG C of -0.05 ~ -0.06 MPa of decompression of temperature are concentrated to give about 17.2 g of 1 finished product of compound.Yield 97.3%, purity
98.5%。ESI: m/z: 167 [M+H]+.
Embodiment 3：The synthesis of compound 1
10.0 g of phenol, 19.6 g of hexamethyldisilazane, 4-dimethylaminopyridine are added into reaction bulb（DMAP） 10.0 g
Unlatching is stirred, 20 ~ 30 DEG C of temperature control, the ammonia generated with cold water absorbing reaction, and after 1.5 h of insulation reaction, reaction terminates, control
Warm 140 ~ 150 DEG C of normal pressures are concentrated to give about 16.9 g of 1 finished product of compound.Yield 95.7%, purity 98.7%.ESI: m/z:
167 [M+H]+.
Embodiment 4：The synthesis of compound 1
10.0 g of phenol, 8.57 g of hexamethyldisilazane, 4-dimethylaminopyridine are added into reaction bulb（DMAP） 0.1 g
Unlatching is stirred, 170 ~ 180 DEG C of temperature control, the ammonia generated with cold water absorbing reaction, and after 1.5 h of insulation reaction, reaction terminates,
30 ~ 40 DEG C of normal pressures of temperature control are concentrated to give about 16.9 g of 1 finished product of compound.Yield 95.7%, purity 98.7%.ESI: m/z:
167 [M+H]+.
Embodiment 5：The synthesis of compound 1
10.0 Kg of phenol, 9.8 Kg of hexamethyldisilazane, 4-dimethylaminopyridine are added into reaction bulb（DMAP） 0.02
Kg, which is opened, to be stirred, 50 ~ 60 DEG C of temperature control, the ammonia generated with cold water absorbing reaction, and after 3 h of insulation reaction, reaction terminates, control
30 ~ 40 DEG C of -0.09 ~ -0.1 MPa of decompression of temperature are concentrated to give about 17.0 Kg of 1 finished product of compound.Yield 96.1%, purity
98.5%。ESI: m/z: 167 [M+H]+.
Embodiment 6：The synthesis of compound 1
30.0 Kg of phenol, 31.0 Kg of hexamethyldisilazane, 4-dimethylaminopyridine are added into reaction bulb（DMAP） 0.03
Kg, which is opened, to be stirred, 20 ~ 30 DEG C of temperature control, the ammonia generated with cold water absorbing reaction, and after 3 h of insulation reaction, reaction terminates, control
30 ~ 40 DEG C of -0.09 ~ -0.1 MPa of decompression of temperature are concentrated to give about 50.5 Kg of 1 finished product of compound.Yield 95.3%, purity
98.9%。ESI: m/z: 167 [M+H]+.
It is of the invention initiative by 4-dimethylaminopyridine（DMAP）Make catalyst to react for this step, obtained trimethylbenzene oxygen
Base silane（Compound 1）Purity is more than 98%, and yield reaches 95% or more, and synthetic method of the invention also has step simple, former
Expect and catalyst is easy to get, production cost is relatively low, toxicity is low, is suitble to industrialized production, waste water few, advantages of environment protection.
Claims (6)
1. a kind of synthetic method of trimethyl phenoxysilane, it is characterised in that include the following steps：
（1）, using phenol and hexamethyldisilazane as raw material, using 4-dimethylaminopyridine as catalyst reaction generate trimethylbenzene
Oxysilane reaction solution；
（2）, after reaction, concentration of reaction solution obtains trimethyl phenoxysilane finished product.
2. a kind of synthetic method of trimethyl phenoxysilane according to claim 1, it is characterised in that step（1）In,
Reaction temperature is：- 20 ~ 180 ℃.
3. a kind of synthetic method of trimethyl phenoxysilane according to claim 1, it is characterised in that step（1）In,
The phenol used is with hexamethyldisilazane mass ratio：1 : 1 ~ 1 : 5.
4. a kind of synthetic method of trimethyl phenoxysilane according to claim 1, it is characterised in that step（1）In,
Phenol is with 4-dimethylaminopyridine mass ratio：1 : 0.0001 ~ 1 : 1.
5. a kind of synthetic method of trimethyl phenoxysilane according to claim 1, it is characterised in that step（2）In,
Thickening temperature is：20 ~ 150 ℃.
6. a kind of synthetic method of trimethyl phenoxysilane according to claim 1, it is characterised in that step（2）In,
Concentrating pressure is：- 0.1 ~0 MPa.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114524839A (en) * | 2022-01-12 | 2022-05-24 | 湖北江瀚新材料股份有限公司 | Preparation method of stearyloxy trimethylsilane |
| CN115028839A (en) * | 2022-07-11 | 2022-09-09 | 桂林宝龙达新材料有限公司 | Preparation method of methyl phenoxy silicone oil |
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| CN115028839A (en) * | 2022-07-11 | 2022-09-09 | 桂林宝龙达新材料有限公司 | Preparation method of methyl phenoxy silicone oil |
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