SU289097A1 - METHOD OF OBTAINING DIALCOXYPHOSPHINES - Google Patents
METHOD OF OBTAINING DIALCOXYPHOSPHINESInfo
- Publication number
- SU289097A1 SU289097A1 SU1380044A SU1380044A SU289097A1 SU 289097 A1 SU289097 A1 SU 289097A1 SU 1380044 A SU1380044 A SU 1380044A SU 1380044 A SU1380044 A SU 1380044A SU 289097 A1 SU289097 A1 SU 289097A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- dialcoxyphosphines
- obtaining
- dialkoxyphosphines
- spectrum
- region
- Prior art date
Links
- XKRFYHLGVUSROY-UHFFFAOYSA-N argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 229910052698 phosphorus Inorganic materials 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- KXOHONQCPYDQTC-UHFFFAOYSA-N chloro(dioxido)phosphane Chemical class [O-]P([O-])Cl KXOHONQCPYDQTC-UHFFFAOYSA-N 0.000 description 2
- YQVYPOYAWKCVIZ-UHFFFAOYSA-N dibutoxyphosphane Chemical compound CCCCOPOCCCC YQVYPOYAWKCVIZ-UHFFFAOYSA-N 0.000 description 2
- 238000002329 infrared spectrum Methods 0.000 description 2
- 125000004437 phosphorous atoms Chemical group 0.000 description 2
- 239000011541 reaction mixture Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- DBGVGMSCBYYSLD-UHFFFAOYSA-N Tributyltin hydride Chemical compound CCCC[SnH](CCCC)CCCC DBGVGMSCBYYSLD-UHFFFAOYSA-N 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- HEIJWSDREXBCOR-UHFFFAOYSA-N chloro-bis(2-methylpropoxy)phosphane Chemical compound CC(C)COP(Cl)OCC(C)C HEIJWSDREXBCOR-UHFFFAOYSA-N 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- KLGZELKXQMTEMM-UHFFFAOYSA-N hydride Chemical compound [H-] KLGZELKXQMTEMM-UHFFFAOYSA-N 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000000543 intermediate Substances 0.000 description 1
- 125000002510 isobutoxy group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])O* 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 125000006606 n-butoxy group Chemical group 0.000 description 1
- 150000002903 organophosphorus compounds Chemical class 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 150000003018 phosphorus compounds Chemical class 0.000 description 1
- 125000002743 phosphorus functional group Chemical group 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing Effects 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N tin hydride Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 229910000083 tin tetrahydride Inorganic materials 0.000 description 1
Description
Изобретение относитс к способу получени диалкоксифосфинов общей формулы (RO)2PH, где R - алкил.This invention relates to a process for the preparation of dialkoxyphosphines of the general formula (RO) 2PH, where R is alkyl.
Эти вещества относ тс к новому классу соединений трехвалентного фосфора, содержащих О-Р и Р-Н св зи. Полученные диалкоксифосфииы перспективны как полупродукты дл синтеза разнообразных фосфорорганических соединений с трехкоординационным атомом фосфора и функциональными группами в молекуле.These substances belong to a new class of trivalent phosphorus compounds containing O-P and P-H bonds. The resulting dialkoxyphosphines are promising as intermediates for the synthesis of various organophosphorus compounds with a three-coordinating phosphorus atom and functional groups in the molecule.
Способ получени диалкоксифосфинов заключаетс в том, что диалкилхлорфосфиты восстанавливают с помощью гидрида триалкилолова в атмосфере инертного газа, например аргона.The method of producing dialkoxyphosphines is that the dialkyl chlorophosphites are reduced with the help of a trialkyltin hydride in an atmosphere of an inert gas, such as argon.
Пример. Все операции провод т в токе сухого аргона. К 29 г гидрида трибутилолова прибавл ют при температуре -10°С 21 г диизобутилхлорфосфита. Через 2 час температуру довод т до комнатной, и выдерживают реакционную смесь при 20°С в течение 2 суток . Затем реакционную смесь подвергают перегонке в вакууме. Получают 13,4 г диизобутоксифосфина . Выход составл ет 75% от теоретического; т. кип. 39°С (1 мм рт. ст.). По 1,4295.-ШExample. All operations are carried out in a stream of dry argon. At 29 ° C, 21 g of diisobutylchlorophosphite was added to 29 g of tributyltin hydride. After 2 hours, the temperature is brought to room temperature, and the reaction mixture is kept at 20 ° C for 2 days. Then the reaction mixture is subjected to distillation in vacuum. 13.4 g of diisobutoxyphosphine are obtained. The yield is 75% of the theoretical; m.p. 39 ° С (1 mm of mercury). According 1.4295.-W
В ИК-спектре имеетс максимум поглощени в области 2210 см (валентные колебани Р-Н св зи).In the IR spectrum, there is an absorption maximum in the region of 2210 cm (stretching vibrations of the P – H bond).
Аналогично получен ди-н-бутоксифосфин. Его выход составл ет 74% от теоретического; т. кип. 49°С (1,5 мм рт. ст.); nf 1,4296.Similarly obtained di-n-butoxyphosphine. Its yield is 74% of theoretical; m.p. 49 ° C (1.5 mmHg); nf 1.4296.
Найдено, %: С 53,99; Н 10,98; Р 17,68.Found,%: C 53.99; H 10.98; R 17.68.
CsHi,OoP.CsHi, OoP.
Вычислено, %: С 53,92; Н 10,75; Р 17,39.Calculated,%: C 53.92; H 10.75; R 17.39.
.В ИК-спектре имеетс максимум поглощени в области 2210 c.. В ПМР-спектре диизобутоксифосфина имеетс симметричный дублет от протона, св занного с атомом фосфора в области 5,17-8,29 м. д. /р-п 199 гц; в ПМР-спектре ди-н-бутоксифосфина - 5,21 - 8,58 м. д., /р-н 199 гц. Соотношение интегральных интенсивностей от протона при фосфоре и протонов соответственно изобутокси-и н-бутоксигрупп составл ет 1 ; 18..In the IR spectrum, there is an absorption maximum in the region of 2210 s. In the PMR spectrum of diisobutoxyphosphine, there is a symmetric doublet from a proton associated with a phosphorus atom in the region of 5.17-8.29 ppm / p-199 Hz; in the PMR spectrum of di-n-butoxyphosphine - 5.21 - 8.58 ppm, / rn 199 Hz. The ratio of the integral intensities of the proton with the phosphorus and the protons, respectively, of the isobutoxy and n-butoxy groups is 1; 18.
Предмет изобретени Subject invention
1.Способ получени диалкоксифосфинов, отличающийс тем, что диалкилхлорфосфит подвергают взаимодействию с гидридом триалкилолова с последующим выделением целевого продукта известными приемами.1. A method for producing dialkoxyphosphines, characterized in that the dialkyl chlorophosphite is reacted with a trialkyl tin hydride, followed by isolation of the target product by known methods.
Publications (1)
| Publication Number | Publication Date |
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| SU289097A1 true SU289097A1 (en) |
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