SU165720A1 - - Google Patents
Info
- Publication number
- SU165720A1 SU165720A1 SU772950A SU772950A SU165720A1 SU 165720 A1 SU165720 A1 SU 165720A1 SU 772950 A SU772950 A SU 772950A SU 772950 A SU772950 A SU 772950A SU 165720 A1 SU165720 A1 SU 165720A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- mol
- chloride
- yield
- temperature
- chlorophosphate
- Prior art date
Links
- ZJEHRMYJNACSLL-UHFFFAOYSA-N 1-[butoxy(chloro)phosphoryl]oxybutane Chemical compound CCCCOP(Cl)(=O)OCCCC ZJEHRMYJNACSLL-UHFFFAOYSA-N 0.000 description 4
- FAIAAWCVCHQXDN-UHFFFAOYSA-N Phosphorus trichloride Chemical compound ClP(Cl)Cl FAIAAWCVCHQXDN-UHFFFAOYSA-N 0.000 description 3
- 238000009835 boiling Methods 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 239000000460 chlorine Substances 0.000 description 3
- 229910052801 chlorine Inorganic materials 0.000 description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- AQSJGOWTSHOLKH-UHFFFAOYSA-N Phosphite Chemical class [O-]P([O-])[O-] AQSJGOWTSHOLKH-UHFFFAOYSA-N 0.000 description 2
- YBBRCQOCSYXUOC-UHFFFAOYSA-N Sulfuryl chloride Chemical compound ClS(Cl)(=O)=O YBBRCQOCSYXUOC-UHFFFAOYSA-N 0.000 description 2
- FYSNRJHAOHDILO-UHFFFAOYSA-N Thionyl chloride Chemical compound ClS(Cl)=O FYSNRJHAOHDILO-UHFFFAOYSA-N 0.000 description 2
- 230000002378 acidificating Effects 0.000 description 2
- 238000007664 blowing Methods 0.000 description 2
- HEDRZPFGACZZDS-UHFFFAOYSA-N chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- BVXOPEOQUQWRHQ-UHFFFAOYSA-N dibutyl phosphite Chemical compound CCCCOP([O-])OCCCC BVXOPEOQUQWRHQ-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- YGYAWVDWMABLBF-UHFFFAOYSA-N phosgene Chemical compound ClC(Cl)=O YGYAWVDWMABLBF-UHFFFAOYSA-N 0.000 description 2
- 235000021317 phosphate Nutrition 0.000 description 2
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N HCl Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 150000001805 chlorine compounds Chemical class 0.000 description 1
- GLUYADGKGBGXRV-UHFFFAOYSA-L chloro phosphate Chemical compound [O-]P([O-])(=O)OCl GLUYADGKGBGXRV-UHFFFAOYSA-L 0.000 description 1
- ITVPBBDAZKBMRP-UHFFFAOYSA-L chloro-dioxido-oxo-$l^{5}-phosphane Chemical class [O-]P([O-])(Cl)=O ITVPBBDAZKBMRP-UHFFFAOYSA-L 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- XYFCBTPGUUZFHI-UHFFFAOYSA-N phosphine Chemical compound P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910000073 phosphorus hydride Inorganic materials 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- -1 thiocyl chloride Chemical compound 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Description
Известен способ получени диалкилхлорфосфатов взаимолействием.хлора или хлористого сульфурила с диалкилфосфитами.A known method of producing dialkyl chlorophosphates by the mutual interaction of chlorine or sulfuryl chloride with dialkyl phosphites.
При осуществлении способа необходимо применение абсолютно сухих реагентов и тщательной защиты от влаги, так как в противном случае образуютс кислые фосфаты, которые разлагают целевые продукты.In carrying out the method, it is necessary to use absolutely dry reagents and careful protection against moisture, since otherwise acidic phosphates are formed, which decompose the target products.
Дл повышени выхода целевого продукта предлагаетс массу после хлорировани обрабатывать реагентами, способными превраа,ать кислые фосфаты в соответстпуюга .ие хлорангидриды, например тионилхлоридом , треххлорисгым фосчфором и хлором, фосгеном, н тихлористым фосфором. Эти реагенты добавл ют в количестве 0,01 - ОЛ моль на 1 ноль фосфита.To increase the yield of the target product, it is proposed to treat the mass after chlorination with reagents capable of converting acidic phosphates to appropriate chlorides, for example, thionyl chloride, trichlorine phosphorus and chlorine, phosphine, and phosphorus chloride. These reagents are added in an amount of 0.01 to OL mol per 1 zero of phosphite.
Пример 1. К 02 моль ;и1бутилфосфита при перемешивании, охлаждении и непрерывном продувании сухого воз;г.уха прибавл ют по капл м 0,22 моль хлористого сульфурил., поддержива температуру реакционной массы в пределах О-5°С. Затем в емесь при перемешивании барботируют 002 моль фосгена, выдерживают при 20°С 3-5 час, снова продувают в течение часа воздух н нерегоикой выдел ют дибутилхлорфосфат с т. кип. 125-127С (10 выход 96% теопетического.Example 1. To 02 mol; i1butylphosphite with stirring, cooling and continuous blowing of dry air, a drop of 0.22 mol of sulfuryl chloride is added dropwise, keeping the temperature of the reaction mass in the range of -5 ° C. Then, 002 mol of phosgene is bubbled into the mixture with stirring, kept at 20 ° C for 3-5 hours, the dibutyl chlorophosphate is recovered from the boil over an hour again, and the boil is stirred. 125-127С (10 is the yield of 96% of theopetic.
CgnisOsPCl.CgnisOsPCl.
В тех же услови х без обработки фосгеном дибутилхлорфосфат получен с выходом УЗо/о. Пример 2. В 0,2 моль дибутилфосфита при перемешивании и охлаждении барботируют хлор до по влени желтой окраски, поддержива температуру не выше 5°С. Затем к смест прибавл ют 0,015 моль треххлористого фосфора и снова хлорируют в тех же усло;л-1 х до желтой окраски. Температуру смесн довод т до компатиой, основную массу хлористого водорода удал ют продуванием сухого поздуха и перегонкой выдел ют дибутилхлорфосфат с т. кип. 127-129°С (11 мм) 1,ыход, теоретического.Under the same conditions, without dibutyl chlorophosphate treatment with phosgene, it was obtained with a yield of UZO / o. Example 2. 0.2 mole of dibutylphosphite is bubbled with stirring and cooling until a yellow color appears, maintaining the temperature not higher than 5 ° C. Then, 0.015 moles of phosphorus trichloride are added to the displacements and again chlorinated under the same conditions; l -1 x to a yellow color. The temperature of the mixture is adjusted to compati, the bulk of the hydrogen chloride is removed by blowing dry dry and the dibutyl chlorophosphate is boiled off with boiling water. 127-129 ° С (11 mm) 1, yield, theoretical.
В а ;алогичных услови х без обработки треххлористым фосфором и хлором дибутилхлорфОсфат нолучеп с выходом .Under aa; illogical conditions, without treatment with phosphorus trichloride and chlorine, dibutylchlorophosphate does not get worse with yield.
Пример 3. Раствор 0., 15 моль дибутилфосфита в двукратном объеме невысушенного хлороформа обрабатывают 0,17 моль хлористого сульоЬурила, а затем 0,015 моль хлористого тиоцила в услови х примера 1.Example 3. Solution of 0., 15 mol of dibutyl phosphite in two times the volume of undried chloroform is treated with 0.17 mol of sulburyl chloride, and then 0.015 mol of thiocyl chloride under the conditions of example 1.
Растворитель и другие низкокип щие продукты отгон ют постенешю повыша темпеpaTyiVv бпдл до 100°С и перегонкой остаткаThe solvent and other low-boiling products are distilled by increasing the temperature of TydyVv bpdl to 100 ° C and distilling the residue.
:;ы;л :)11(;т .чхлорфосфат с т. кип. 25 -:;; s; l:) 11 (; t. chlorophosphate with bp 25 -
Publications (1)
| Publication Number | Publication Date |
|---|---|
| SU165720A1 true SU165720A1 (en) |
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