SU210155A1 - METHOD OF OBTAINING 1-CHLOR-3,4-BENZOPHOSPHOLINE - Google Patents
METHOD OF OBTAINING 1-CHLOR-3,4-BENZOPHOSPHOLINEInfo
- Publication number
- SU210155A1 SU210155A1 SU1110515A SU1110515A SU210155A1 SU 210155 A1 SU210155 A1 SU 210155A1 SU 1110515 A SU1110515 A SU 1110515A SU 1110515 A SU1110515 A SU 1110515A SU 210155 A1 SU210155 A1 SU 210155A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- benzophospholine
- chlor
- obtaining
- chloro
- heating
- Prior art date
Links
- FMGGHNGKHRCJLL-UHFFFAOYSA-N 1,2-bis(chloromethyl)benzene Chemical compound ClCC1=CC=CC=C1CCl FMGGHNGKHRCJLL-UHFFFAOYSA-N 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 3
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 claims description 3
- 229910052740 iodine Inorganic materials 0.000 claims description 3
- 239000011630 iodine Substances 0.000 claims description 3
- XYFCBTPGUUZFHI-UHFFFAOYSA-N phosphine Chemical compound P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 claims description 3
- 230000003197 catalytic Effects 0.000 claims description 2
- 150000004694 iodide salts Chemical class 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- FAIAAWCVCHQXDN-UHFFFAOYSA-N Phosphorus trichloride Chemical compound ClP(Cl)Cl FAIAAWCVCHQXDN-UHFFFAOYSA-N 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- VZGDMQKNWNREIO-UHFFFAOYSA-N Carbon tetrachloride Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000000875 corresponding Effects 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 230000000749 insecticidal Effects 0.000 description 1
- 239000002917 insecticide Substances 0.000 description 1
- 239000010687 lubricating oil Substances 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
- 239000000203 mixture Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 235000015149 toffees Nutrition 0.000 description 1
Description
Насто щее изобретение касаетс способа получени 1-хлор-3,4-бензофосфолина общей формулыThe present invention relates to a process for the preparation of 1-chloro-3,4-benzophospholine of the general formula
HjCkpJCHjHjckpjchj
С1C1
Соединение может быть использовано в качестве исходного вещества дл получени инсектицидов , экстрагентов, ирисадок к смазочным маслам и т. д.The compound can be used as a starting material for the preparation of insecticides, extractants, toffee to lubricating oils, etc.
Предлагаемый способ состоит в том, что белый фосфор подвергают взаимодействию с о-ксилилендихлоридом при нагревании желательно до 270-280°С в присутствии каталитических количеств йода или йодидов и треххлористого фосфора в качестве растворител .The proposed method consists in the fact that white phosphorus is reacted with o-xylylene dichloride with heating preferably up to 270-280 ° C in the presence of catalytic amounts of iodine or iodides and phosphorus trichloride as a solvent.
Пример. Получение 1-хлор-3,4-бензофосфолина .Example. Preparation of 1-chloro-3,4-benzophospholine
Смесь 0,086 г-моль о-ксилилендихлорида, 0,097 г-атм. белого фосфора, 0,507 г-моль треххлористого фосфора и 0,2 г йода нагревают в автоклавной пробирке при температуре 270-280° С в течение 8 час. Треххлористый фосфор и избыток о-ксилилендихлорида отгон ют и перегонкой выдел ют 6,7 г 1-хлор-3,4-бензофосфолина . Выход 54,4о/о т. кип. 124- 125° С (2,5 .иж рт. ст., т. пл.48-49°С. Найдено, %: С1 20,5, 20,9; Р 18,40, 18,73.A mixture of 0.086 g-mol o-xylylene dichloride, 0.097 g-atm. white phosphorus, 0.507 g-mol of phosphorus trichloride and 0.2 g of iodine are heated in an autoclave tube at a temperature of 270-280 ° C for 8 hours. Phosphorus trichloride and excess o-xylylene dichloride are distilled off and 6.7 g of 1-chloro-3,4-benzophospholine is isolated by distillation. Output 54,4o / o T. Kip. 124-125 ° C (2.5 .zhi mercury., T. Square 48-49 ° C. Found,%: C1 20.5, 20.9; P 18.40, 18.73.
CgHsClPCgHsClP
Вычислено, й/д: С1 20,8; Р 18,16.Calculated y / d: C1 20.8; P 18.16.
1-хлор-3,4-бензофосфолин гидролизуют с количественным выходом в соответствующую о-ксилиленфосфиновую кислоту - кристаллическое вещество белого цвега, перекристаллизовывают из четыреххлористого углерода. Т. пл. 137-140° С.1-chloro-3,4-benzophospholine is hydrolyzed with a quantitative yield to the corresponding o-xylylenephosphinic acid — a white crystalline crystalline substance, recrystallized from carbon tetrachloride. T. pl. 137-140 ° C.
Найдено, «/о: С 55,92, 55,27; Н 5,30, 5,53; Р 18,01, 18,16.Found, “/ o: C 55.92, 55.27; H 5.30, 5.53; P 18.01, 18.16.
CsHgOaP.CsHgOaP.
Вычислено, %: С 56,80; Н 5,36; Р 18,45.Calculated,%: C 56.80; H 5.36; R 18.45.
Предмет изобретени Subject invention
Claims (2)
Publications (1)
| Publication Number | Publication Date |
|---|---|
| SU210155A1 true SU210155A1 (en) |
Family
ID=
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3723520A (en) * | 1971-06-01 | 1973-03-27 | Upjohn Co | Process for the preparation of 1-halophospholenes |
| US3723521A (en) * | 1971-06-01 | 1973-03-27 | Upjohn Co | Process for the preparation of 1-halophospholenes |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3723520A (en) * | 1971-06-01 | 1973-03-27 | Upjohn Co | Process for the preparation of 1-halophospholenes |
| US3723521A (en) * | 1971-06-01 | 1973-03-27 | Upjohn Co | Process for the preparation of 1-halophospholenes |
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