SU179770A1 - METHOD OF OBTAINING SILICON CONTAINING PEROXIDE COMPOUNDS - Google Patents
METHOD OF OBTAINING SILICON CONTAINING PEROXIDE COMPOUNDSInfo
- Publication number
- SU179770A1 SU179770A1 SU931668A SU931668A SU179770A1 SU 179770 A1 SU179770 A1 SU 179770A1 SU 931668 A SU931668 A SU 931668A SU 931668 A SU931668 A SU 931668A SU 179770 A1 SU179770 A1 SU 179770A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- silicon containing
- mol
- peroxide compounds
- containing peroxide
- obtaining silicon
- Prior art date
Links
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title description 5
- 229910052710 silicon Inorganic materials 0.000 title description 5
- 239000010703 silicon Substances 0.000 title description 3
- -1 PEROXIDE COMPOUNDS Chemical class 0.000 title description 2
- VLKZOEOYAKHREP-UHFFFAOYSA-N hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 10
- JUJWROOIHBZHMG-UHFFFAOYSA-N pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 6
- 239000008079 hexane Substances 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- BLRPTPMANUNPDV-UHFFFAOYSA-N silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 3
- 229910000077 silane Inorganic materials 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 230000002194 synthesizing Effects 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 125000000217 alkyl group Chemical group 0.000 description 2
- 125000003710 aryl alkyl group Chemical group 0.000 description 2
- UHOVQNZJYSORNB-UHFFFAOYSA-N benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 2
- CSNNHWWHGAXBCP-UHFFFAOYSA-L mgso4 Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 2
- AOJFQRQNPXYVLM-UHFFFAOYSA-N pyridin-1-ium;chloride Chemical compound [Cl-].C1=CC=[NH+]C=C1 AOJFQRQNPXYVLM-UHFFFAOYSA-N 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- ZXXAWPIEDDWXHD-UHFFFAOYSA-N tert-butylperoxymethanol Chemical compound CC(C)(C)OOCO ZXXAWPIEDDWXHD-UHFFFAOYSA-N 0.000 description 2
- JLUFWMXJHAVVNN-UHFFFAOYSA-N Methyltrichlorosilane Chemical compound C[Si](Cl)(Cl)Cl JLUFWMXJHAVVNN-UHFFFAOYSA-N 0.000 description 1
- IJOOHPMOJXWVHK-UHFFFAOYSA-N Trimethylsilyl chloride Chemical compound C[Si](C)(C)Cl IJOOHPMOJXWVHK-UHFFFAOYSA-N 0.000 description 1
- YLJJAVFOBDSYAN-UHFFFAOYSA-N dichloro-ethenyl-methylsilane Chemical compound C[Si](Cl)(Cl)C=C YLJJAVFOBDSYAN-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 239000012442 inert solvent Substances 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 229910052943 magnesium sulfate Inorganic materials 0.000 description 1
- 235000019341 magnesium sulphate Nutrition 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 239000005055 methyl trichlorosilane Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000012044 organic layer Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 125000002081 peroxide group Chemical group 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000005051 trimethylchlorosilane Substances 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
Description
Кремнийсодержащие перекисные соединени , в которых перекисна группа не св зана непосредственно с атомом кремни , не описаны . Предложен способ получени указанных соединений , заключающийс в том, что алкил (аралкил)пероксналканолы подвергают взаимодействию с галоидсиланами. Процесс провод т при -20 - 40° С в присутствии основани в среде инертного органического растворител , например гексана. Строение полученных соединений доказываетс физико-химическими данными. Пример 1. Синтез триметил(т/ ег-бутилпероксиметилокси )силана. К охлажденному до -5° С раствору 7,03 г (0,065 моль) триметилхлорсилана в 50 мл гексана по капл м при перемешивании прибавл ют смесь 7,8 г (0,065 моль) трет-бутилпероксиметанола и 5,15 г (0,065 моль) пиридина в 50 мл гексана. Температура во врем прикапывани не превыщала 0° С. После перемешивани реакционной смеси в течение 3 час при комнатной температуре хлоргидрат пиридина раствор ют в небольшом количестве воды и отдел ют. Органический слой промывают водой, 25%-ным спиртом, снова водой и сушат сульфатом магни . Затем удал ют растворитель в вакууме и выдерживают продукт в бане при 50° С (1 мм рт. ст.). Получают 9,6 г (77%) вещеста с ng 1,4045, df 0,8788. Найдено в %: С 50,36; Н 10,57; Si 14,38, акт 8,42. CsHaoSiOs. : С 49,96, Н 10,48, Si 14,60, Вычислено в Оакт 8,33. Пример 2. Синтез метилтри (грег-бутилпероксиметилокси )силана. Из 3,75 г (0,025 моль) метилтрихлорсилана, 9,12 г (0,076 моль), грег-бутилпероксиметанола и 6,1 г (0,076 моль) пиридина в 60 мл бензола в услови х примера 1 получают 8,5 г (85о/о) вещества с 1,4225, df 1,0113. Найдено в о/о. С 48,04; Н 9,13; Si 6,92; О акт 11,85. CioHseSiOg. Вычислено в %: С 47,98; Н 9,06; Si 7,01; Оакт 11,98. Пример 3. Синтез метилвинилди(трег-бутилпероксиметилокси )силана. Из 5,28 г (0,0375 моль) метилвинилдихлорсилана, 9 (0,075 моль) трет-бутилпероксиметанола и 5,95 г (0,075 моль) пиридина в 60 мл гексана в услови х примера 1 получают 9,3 г (800/0) вещества с ng 1,4300, df 0,9779. О Silicon-containing peroxide compounds in which the peroxide group is not bound directly to the silicon atom are not described. A method for the preparation of these compounds is proposed, in which the alkyl (aralkyl) peroxynol alkanols are reacted with halosilanes. The process is carried out at -20 - 40 ° C in the presence of a base in an environment of an inert organic solvent, for example hexane. The structure of the compounds obtained is proved by physicochemical data. Example 1. Synthesis of trimethyl (t / E-butylperoxymethyl) silane. To a solution of 7.03 g (0.065 mol) of trimethylchlorosilane in 50 ml of hexane cooled to -5 ° C, a mixture of 7.8 g (0.065 mol) of tert-butyl peroxymethanol and 5.15 g (0.065 mol) of pyridine was added dropwise with stirring in 50 ml of hexane. The temperature during the dropping was no higher than 0 ° C. After stirring the reaction mixture for 3 hours at room temperature, pyridine hydrochloride was dissolved in a small amount of water and separated. The organic layer is washed with water, 25% alcohol, again with water, and dried with magnesium sulfate. The solvent is then removed in vacuo and the product is kept in a bath at 50 ° C (1 mm Hg). 9.6 g (77%) of the substance are obtained with ng 1.4045, df 0.8788. Found in%: C 50.36; H 10.57; Si 14.38, Act 8.42. CsHaoSiOs. : C 49.96, H 10.48, Si 14.60, Calculated at Oact 8.33. Example 2. Synthesis of methyltri (Greg-butylperoxymethyl) silane. From 3.75 g (0.025 mol) of methyl trichlorosilane, 9.12 g (0.076 mol), Greg-butyl peroxymethanol and 6.1 g (0.076 mol) of pyridine in 60 ml of benzene under the conditions of example 1, 8.5 g (85 ° / o) substances with 1.4225, df 1.0113. Found in oo. C 48.04; H 9.13; Si 6.92; O Act 11.85. CioHseSiOg. Calculated in%: C 47.98; H 9.06; Si 7.01; Oact 11.98. Example 3. Synthesis of methylvinyldi (treg-butylperoxymethyl) silane. Out of 5.28 g (0.0375 mol) of methyl vinyl dichlorosilane, 9 (0.075 mol) of tert-butyl peroxymethanol and 5.95 g (0.075 mol) of pyridine in 60 ml of hexane under conditions of example 1, 9.3 g (800/0) are obtained. substances with ng 1,4300, df 0,9779. ABOUT
Вычислено Б %: С 50,62; Н 9,15; Si 9,11; ОакПО,38.Calculated B%: C 50.62; H 9.15; Si 9.11; OakPO, 38.
Полученные соединени смогут найти применение в качестве инициаторов полимеризации винильных соединений, а также дл других целей.The resulting compounds can be used as initiators for the polymerization of vinyl compounds, as well as for other purposes.
Предмет изобретени Subject invention
Способ получени кремнийсодержащих иерекисных соединений, в которых перекисна The method of obtaining silicon-containing irekisnyh compounds in which the peroxide
группа не св зана непосредственно с атомо.м кремни , отличающийс тем, что алкил(аралкил )иероксиалкаполь подвергают взаимодейств )1Ю с органическими галоидсиланами в присутствии основани в среде инертного растворител , например гексана, при температуре -20 -40° С.the group is not directly bonded to silicon atom, characterized in that the alkyl (aralkyl) ieroxyalkapole is reacted with organic halo-silanes in the presence of a base in an inert solvent, for example hexane, at -20 -40 ° C.
Publications (1)
| Publication Number | Publication Date |
|---|---|
| SU179770A1 true SU179770A1 (en) |
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