SU207912A1 - METHOD OF OBTAINING SILICON ORGANIC ACETALS - Google Patents
METHOD OF OBTAINING SILICON ORGANIC ACETALSInfo
- Publication number
- SU207912A1 SU207912A1 SU1094596A SU1094596A SU207912A1 SU 207912 A1 SU207912 A1 SU 207912A1 SU 1094596 A SU1094596 A SU 1094596A SU 1094596 A SU1094596 A SU 1094596A SU 207912 A1 SU207912 A1 SU 207912A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- silicon organic
- acetals
- obtaining silicon
- alkyl ethers
- ether
- Prior art date
Links
- 150000001241 acetals Chemical class 0.000 title claims description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title 1
- 229910052710 silicon Inorganic materials 0.000 title 1
- 239000010703 silicon Substances 0.000 title 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 239000003054 catalyst Substances 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 150000004819 silanols Chemical class 0.000 claims description 3
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 229920001296 polysiloxane Polymers 0.000 claims description 2
- 150000005215 alkyl ethers Chemical class 0.000 claims 2
- 238000000034 method Methods 0.000 claims 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 8
- -1 propyl triethylsilyl Chemical group 0.000 description 2
- SCPYDCQAZCOKTP-UHFFFAOYSA-N silanol Chemical compound [SiH3]O SCPYDCQAZCOKTP-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- VHUQXPJHMISKGS-UHFFFAOYSA-N 1-(chloromethoxy)propane Chemical compound CCCOCCl VHUQXPJHMISKGS-UHFFFAOYSA-N 0.000 description 1
- 239000007832 Na2SO4 Substances 0.000 description 1
- 230000002378 acidificating Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- HEDRZPFGACZZDS-UHFFFAOYSA-N chloroform Substances ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 1
- 125000005670 ethenylalkyl group Chemical group 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing Effects 0.000 description 1
- WVMSIBFANXCZKT-UHFFFAOYSA-N triethyl(hydroxy)silane Chemical compound CC[Si](O)(CC)CC WVMSIBFANXCZKT-UHFFFAOYSA-N 0.000 description 1
- 238000005292 vacuum distillation Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Description
Известен способ получени кремнийорганических ацеталей взаимодействием силанолов с винилалкиловыми эфирами в присутствии кислого катализатора.A known method for producing silicone acetals by reacting silanols with vinyl alkyl ethers in the presence of an acidic catalyst.
С целью расширени сырьевой базы, предложено силанолы подвергать взаимодействию с а-хлорметилалкиловыми эфирами в присутствии едкого натра при охлаждении до Он4°С.In order to expand the resource base, it is proposed to react silanols with a-chloromethyl alkyl ethers in the presence of caustic soda while cooling to 4 ° C.
Синтез н. пропилтриэтилсилилформал .Synthesis n. propyl triethylsilyl formal.
В трехгорлую колбу емкостью 150 мл, снабженную механической мешалкой, обратным холодильником, двум капельными воронками и термометром внос т 2 г NaOH и 50 мл абсолютного эфира. В первую капельную воронку наливают 11 г -хлорметилпропилового эфира, растворенного в 10 мл сухого эфира, во вторую-13 г триэтилсиланола, растворенного в 10 мл сухого эфира. При посто нном перемешивании и охлаждении до -4°С в реакционную колбу прикапывают несколько капель а-хлорметилпропилового эфира. Через 2 мин дают еще несколько капель эфирного раствора силанола. По окончании подачи а-хлорэфира и силанола смесь нагревают в течение 3 час на вод ной бане. При этом выдел етс обильный белый осадок (NaCl), который отфильтровывают, фильтрат сушат над безводным Na2S04. После отгонки эфира вакуумной перегонкой выдел ют 8,3 г (41,5%) н.пропилтриэтилсилилформал - н.In a three-necked flask with a capacity of 150 ml, equipped with a mechanical stirrer, a reflux condenser, two dropping funnels and a thermometer, 2 g of NaOH and 50 ml of absolute ether are added. 11 g of chloromethylpropyl ether dissolved in 10 ml of dry ether are poured into the first dropping funnel, and 13 g of triethylsilanol dissolved in 10 ml of dry ether are added to the second dropping funnel. With constant stirring and cooling to -4 ° C, a few drops of a-chloromethylpropyl ether are added dropwise to the reaction flask. After 2 minutes, give a few more drops of the ethereal silanol solution. After the end of the supply of a-chloroform and silanol, the mixture is heated for 3 hours in a water bath. This gives off a rich white precipitate (NaCl), which is filtered off, the filtrate is dried over anhydrous Na2SO4. After the ether was distilled off by vacuum distillation, 8.3 g (41.5%) of n. Propyltriethylsilylformal - n was isolated.
СзН70СНа051(С2Н5)з.SzN70SNa051 (C2H5) h.
d4 0,8672;d4 0.8672;
Т. кип. 76-78°С/5 мм рт. ст.; п 1,4278; MRo найдено 60,57; вычислено 60,80.T. Kip. 76-78 ° C / 5 mm Hg. v .; p 1.4278; MRo found 60.57; calculated 60.80.
Вычислено, о/о: С 58,76; Н 11,83; Si 13,74.Calculated, o / o: C 58.76; H 11.83; Si 13.74.
Найдено, 7о: С 59,06; 59,16; Н 12,02; 12,24; Si 13,28; 13,42.Found 7 °: C 59.06; 59.16; H 12.02; 12.24; Si 13.28; 13.42.
Аналогично получены н. бутилтриэтилсилилформаль с т. кип. 95-97°С/8 мм рт. ст. и н. бутилдиэтилфенилсилилформаль с т. кип. 155-156°С/2 мм рт. ст.Similarly obtained n. butyltriethylsilyformal with t. Kip. 95-97 ° C / 8 mm Hg. Art. and n. butyldiethylphenylsilyl formal with t. Kip. 155-156 ° C / 2 mmHg Art.
Предмет изобретени Subject invention
Claims (2)
Publications (1)
| Publication Number | Publication Date |
|---|---|
| SU207912A1 true SU207912A1 (en) |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4482729A (en) * | 1984-03-04 | 1984-11-13 | Daikin Kogyo Co., Ltd. | Fluoroalkyl silyl ketene acetals and a process for preparing the same |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4482729A (en) * | 1984-03-04 | 1984-11-13 | Daikin Kogyo Co., Ltd. | Fluoroalkyl silyl ketene acetals and a process for preparing the same |
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