SU179313A1 - METHOD FOR OBTAINING HEXAALKYLTRRIAMIDOALKYLPHOSPHONY THIOPHOSPHATES - Google Patents
METHOD FOR OBTAINING HEXAALKYLTRRIAMIDOALKYLPHOSPHONY THIOPHOSPHATESInfo
- Publication number
- SU179313A1 SU179313A1 SU924911A SU924911A SU179313A1 SU 179313 A1 SU179313 A1 SU 179313A1 SU 924911 A SU924911 A SU 924911A SU 924911 A SU924911 A SU 924911A SU 179313 A1 SU179313 A1 SU 179313A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- thiophosphates
- hexaalkyltrriamidoalkylphosphony
- obtaining
- alkyl
- petroleum ether
- Prior art date
Links
- 125000000217 alkyl group Chemical group 0.000 description 6
- RTZKZFJDLAIYFH-UHFFFAOYSA-N diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 6
- 239000003208 petroleum Substances 0.000 description 3
- RYYWUUFWQRZTIU-UHFFFAOYSA-K thiophosphate Chemical class [O-]P([O-])([O-])=S RYYWUUFWQRZTIU-UHFFFAOYSA-K 0.000 description 3
- 125000003118 aryl group Chemical group 0.000 description 2
- UHOVQNZJYSORNB-UHFFFAOYSA-N benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 125000004185 ester group Chemical group 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- -1 o-methyl-ethyl-2, 4,5-trichlorophenyl thiophosphate Chemical compound 0.000 description 1
- 150000002903 organophosphorus compounds Chemical class 0.000 description 1
- RYYWUUFWQRZTIU-UHFFFAOYSA-N thiophosphoric acid Chemical compound OP(O)(S)=O RYYWUUFWQRZTIU-UHFFFAOYSA-N 0.000 description 1
Description
Предложен способ получени нового класса фосфорорганических соединений тиофосфатов гексаалкилтриамидоалкилфосфони общей формулы. 0-P-OR (КзК)зР OR где R - алкил, R - низший алкил, R - алкил , арил или сложноэфирна группировка, взаимодействием гексаалкилтриамидофосфинов с эфирами тиофосфорной кислоты. Пример: К раствору 0,01 моль о-метило-этил-2 ,4,5-трихлорфенилтиофосфата в 10 мл сухого петролейного эфира прибавл ют в токе азота 0,01 моль гекса-н-пропилтриамидофосфина . Полученную смесь помещают в цилиндр с притертой пробкой и выдерживают в атмосфере азота при комнатной температуре в течение трех дней. За это врем в результате реакции образуетс амидофосфониевое соединение, нерастворимое в петролейном эфире, которое выдел етс из реакционного раствора в виде прозрачного масла. Затем соединение собирают, раствор ют в 2-3 мл абс. бензола и высаживают петролейным эфиром. Операцию повтор ют дважды. Растворитель отдел ют, переосажденпое масло выдерживают в вакууме при 15 мм рт. ст. и температуре 50-60°С в течение 10-15 мин. Дл полного удалени остатка растворител масло выдерживают в высоком вакууме при 0,15 мм рт. ст. и . Получают о-этнл-о-2, 4,5-трихлорфенилтнофосфат Р-метил-Р-гекса .и-пропилтриаминофосфони с выходом 33%; D 1,5295; d 4 1,889. Подобным образом получают тиофосфаты гексаалкилтриамидоалкилфосфоии , константы которых приведены в таблице. Предмет изобретени Способ получени тиофосфатов гексаалкилтриамидоалкилфосфони общей формулы 0-P-OR OR где R - алкил, R-низший алкил, R - алкил , арил или сложноэфирна группировка, отличающийс тем, что эфиры тиофосфорной кислоты подвергают взаимодействию с гексаалкилтриамидофосфинами .A method is proposed for producing a new class of organophosphorus compounds of hexaalkyltriamidoalkylphosphonium thiophosphates of the general formula. Where R is alkyl, R is lower alkyl, R is alkyl, aryl or ester group, by reacting hexaalkyltriamidophosphines with thiophosphoric esters. Example: To a solution of 0.01 mol of o-methyl-ethyl-2, 4,5-trichlorophenyl thiophosphate in 10 ml of dry petroleum ether, 0.01 mol of hexa-n-propyltriamidophosphine was added in a stream of nitrogen. The resulting mixture is placed in a cylinder with a ground in stopper and kept in a nitrogen atmosphere at room temperature for three days. During this time, the reaction produces an amidophosphonium compound, insoluble in petroleum ether, which is isolated from the reaction solution as a clear oil. The compound is then collected, dissolved in 2-3 ml of abs. benzene and planted with petroleum ether. The operation is repeated twice. The solvent is separated, the re-precipitated oil is kept under vacuum at 15 mm Hg. Art. and a temperature of 50-60 ° C for 10-15 minutes. To completely remove the residual solvent, the oil is kept under high vacuum at 0.15 mm Hg. Art. and O-ethnl-o-2, 4,5-trichlorophenylphosphate P-methyl-P-hexa and -propyltriaminophosphonium is obtained with a yield of 33%; D 1.5295; d 4 1,889. Thiophosphates of hexaalkyltriamidoalkylphosphoias are obtained in a similar way, the constants of which are given in the table. The subject of the invention is a method for producing hexaalkyltriamidoalkylphosphonium thiophosphates of the general formula 0-P-OR OR where R is alkyl, R-lower alkyl, R is alkyl, aryl or ester group, characterized in that the esters of thiophosphoric acid are reacted with hexaalkyltriamidophosphines.
Publications (1)
Publication Number | Publication Date |
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SU179313A1 true SU179313A1 (en) |
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