SU302345A1 - CLIENT I - Google Patents
CLIENT IInfo
- Publication number
- SU302345A1 SU302345A1 SU1332775A SU1332775A SU302345A1 SU 302345 A1 SU302345 A1 SU 302345A1 SU 1332775 A SU1332775 A SU 1332775A SU 1332775 A SU1332775 A SU 1332775A SU 302345 A1 SU302345 A1 SU 302345A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- product
- phosphorus
- yield
- distilled
- chloroethylphosphonic acid
- Prior art date
Links
- 239000000047 product Substances 0.000 description 5
- RBTARNINKXHZNM-UHFFFAOYSA-K Iron(III) chloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 3
- AQSJGOWTSHOLKH-UHFFFAOYSA-N Phosphite Chemical compound [O-]P([O-])[O-] AQSJGOWTSHOLKH-UHFFFAOYSA-N 0.000 description 3
- FAIAAWCVCHQXDN-UHFFFAOYSA-N Phosphorus trichloride Chemical compound ClP(Cl)Cl FAIAAWCVCHQXDN-UHFFFAOYSA-N 0.000 description 3
- IIMIOEBMYPRQGU-UHFFFAOYSA-L Picoplatin Chemical compound N.[Cl-].[Cl-].[Pt+2].CC1=CC=CC=N1 IIMIOEBMYPRQGU-UHFFFAOYSA-L 0.000 description 3
- 238000006317 isomerization reaction Methods 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- UHZYTMXLRWXGPK-UHFFFAOYSA-N Phosphorus pentachloride Chemical compound ClP(Cl)(Cl)(Cl)Cl UHZYTMXLRWXGPK-UHFFFAOYSA-N 0.000 description 2
- XHXFXVLFKHQFAL-UHFFFAOYSA-N Phosphoryl chloride Chemical compound ClP(Cl)(Cl)=O XHXFXVLFKHQFAL-UHFFFAOYSA-N 0.000 description 2
- 230000003197 catalytic Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- WSLDOOZREJYCGB-UHFFFAOYSA-N 1,2-dichloroethane Chemical compound ClCCCl WSLDOOZREJYCGB-UHFFFAOYSA-N 0.000 description 1
- UDPGUMQDCGORJQ-UHFFFAOYSA-N Ethephon Chemical compound OP(O)(=O)CCCl UDPGUMQDCGORJQ-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000012043 crude product Substances 0.000 description 1
- 229940042400 direct acting antivirals Phosphonic acid derivatives Drugs 0.000 description 1
- IAYPIBMASNFSPL-UHFFFAOYSA-N oxane Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 1
- 150000003007 phosphonic acid derivatives Chemical class 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000011541 reaction mixture Substances 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
- MJNHIYILRDOOTC-UHFFFAOYSA-N tetrachlorophosphanium Chemical compound Cl[P+](Cl)(Cl)Cl MJNHIYILRDOOTC-UHFFFAOYSA-N 0.000 description 1
Description
Изобретение касаетс получени производных фосфоновых кислот. Предлагаетс ) способ получени дихлорангидрида р-хлорэтилфосфоновой кислоты - важнейшего полупродукта синтеза фосфорорганических полимеров .The invention relates to the preparation of phosphonic acid derivatives. A method is proposed for the preparation of p-chloroethylphosphonic acid dichloride, an essential intermediate in the synthesis of organophosphorus polymers.
Известен способ получени дихлорангидрида р-хлорэтилфосфоновой кислоты взаимодействием продукта термической изомеризации тр«с-(р-хлорэтил) фосфита (полученного и а треххлористого фосфора и окиси этилена) с п тихлористым фосфором нри 140-150°С п присутствии каталитических количеств хлорного железа. Выход 65-70%.A known method for the preparation of p-chloroethylphosphonic acid dichloride is obtained by reacting the thermal isomerization product of tr ' c- (p-chloroethyl) phosphite (obtained with phosphorus trichloride and ethylene oxide) with phosphorus tetrachloride at 140-150 ° C in the presence of catalytic ferric chloride. Yield 65-70%.
С целью повышени выхода продукта, предлагаетс процесс проводить при 110-130°С. Выход очищенного перегонкой дихлорангидрида р-хлорэтилфосфоновой кислоты 90-95%.In order to increase the yield of the product, the process is proposed to be carried out at 110-130 ° C. The yield of distilled distilled p-chloroethylphosphonic acid dichloride is 90-95%.
Пример. В сыром продукте термической изомеризации г/7ыс-(р-хлорэтил)фосфита, полученном известным способом из 700 мл (1100 г, 8 г-моль) треххлорпстого фосфора, раствор ют 16,8 г безводного хлорного железа . Температуру раствора довод т до 110°С и к нему при перемешивании порци ми сначала по 100 г, потом до 300 г подсыпают 3300 гExample. In a crude product of thermal isomerization, g / 7ys- (p-chloroethyl) phosphite, obtained in a known manner from 700 ml (1100 g, 8 g-mol) of trichlorophosphorus, 16.8 g of anhydrous ferric chloride is dissolved. The temperature of the solution is adjusted to 110 ° C and, with stirring, portions of 100 g each are added first, then 3300 g are added to 300 g
(7,9 г-моль) п тихлористого фосфора с такими интервалами, чтобы спокойно отгон лись образующиес дихлорэтан п хлорокись фосфора . Температуру к концу добавлени довод т до 120-125 С и после его окончани до 130°С. Всего на добавление п тихлористого фосфора и на нагревание до 130°С требуетс 3,5 час. Далее реакционную смесь охлаждают и перегон ют в вакууме, что дает 1360 г (93,7%) дпхлорангидрида р-хлорэтилфосфоновой кислоты с т. кип. 104°С/11 мм рг. ст.;(7.9 g-mol) of phosphorus chloride at such intervals that the dichloroethane and phosphorus oxychloride are quietly distilled off. The temperature at the end of the addition is adjusted to 120-125 ° C and, after its termination, to 130 ° C. A total of 3.5 hours is required for the addition of phosphorus pentachloride and for heating to 130 ° C. Next, the reaction mixture is cooled and distilled in vacuo, which gives 1360 g (93.7%) of p-chloroethylphosphonic acid dchlorohydride with m.p. 104 ° C / 11 mm rg. v .;
п2о 1,4970.p2o 1.4970.
Предмет изобретени Subject invention
1515
Способ получени дихлорангндрнда Р-хлорэтилфосфоновой кислоты взаимодействием продукта термической изомеризации грнс-(рхлорэтил ) фосфита с п тихлористым фосфором при нагревани) в присутствии каталитических количеств хлорного железа с иоследующим выделением целевого продукта известными приемами, отличающийс тем, что, с цельюThe method of producing P-chloroethylphosphonic acid dichlorangndrna by reacting the UAH-(phloroethyl) phosphite thermal isomerization product with phosphorus pentachloride by heating) in the presence of catalytic amounts of ferric chloride with the subsequent release of the target product by known methods, characterized in that
повыщени выхода продукта, процесс провод т при 110-130 С.increase the yield of the product, the process is carried out at 110-130 C.
Publications (1)
| Publication Number | Publication Date |
|---|---|
| SU302345A1 true SU302345A1 (en) |
Family
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