SU213865A1 - METHOD OF OBTAINING 2,2'-DIAMINODETHYL ETHER OF TETRAMETHYL SPHINIC ACID - Google Patents
METHOD OF OBTAINING 2,2'-DIAMINODETHYL ETHER OF TETRAMETHYL SPHINIC ACIDInfo
- Publication number
- SU213865A1 SU213865A1 SU1045657A SU1045657A SU213865A1 SU 213865 A1 SU213865 A1 SU 213865A1 SU 1045657 A SU1045657 A SU 1045657A SU 1045657 A SU1045657 A SU 1045657A SU 213865 A1 SU213865 A1 SU 213865A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- acid
- ether
- obtaining
- diaminodethyl
- tetramethyl
- Prior art date
Links
- 239000002253 acid Substances 0.000 title claims description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N HCl Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- 150000002148 esters Chemical class 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- AOASVTBKGBXGTN-UHFFFAOYSA-N OP(=O)CCl Chemical compound OP(=O)CCl AOASVTBKGBXGTN-UHFFFAOYSA-N 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 claims description 2
- 239000011541 reaction mixture Substances 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 claims 1
- 230000001376 precipitating Effects 0.000 claims 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- RTZKZFJDLAIYFH-UHFFFAOYSA-N diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- -1 2,2-diamino ethyl Chemical group 0.000 description 1
- 230000002378 acidificating Effects 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 239000008139 complexing agent Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
Description
Предложен способ получени тетраметплфосфиновой кислоты 2,2-диампнодиэтилового эфира.A method for the preparation of tetramethylphosphinic acid 2,2-dipododiethyl ester has been proposed.
Полученное соединение может быть использовано в качестве комплексообразовател .The compound obtained can be used as a complexing agent.
Предлагаемый способ состоит в том, что 2,2-диаминодиэтиловый эфир подвергают взаимодействию с хлорметилфосфиновой кислотой при нагревании до 108-110°С в щелочной среде в токе азота с последующим выделением целевого продукта добавлением в полученную при этом реакционную массу сол ной кислоты и осаждением целевого продукта избытком метанола.The proposed method consists in that the 2,2-diaminodiethyl ether is reacted with chloromethylphosphinic acid when heated to 108-110 ° C in an alkaline medium in a stream of nitrogen, followed by separation of the target product by adding hydrochloric acid to the resulting reaction mass product in excess of methanol.
Пример. Получение тетраметилфосфиновой кислоты 2,2-диаминодиэтилового эфира.Example. Obtaining tetramethylphosphinic acid 2,2-diaminodiethyl ether.
156,6 г (1,2 моль) хлорметплфосфиновой кислоты раствор ют в 75 мл дистиллированной воды, нейтрализуют 40%-ным едким натром (96 г едкого натра в 144 мл дистиллированной воды) и добавл ют 47 г безводного углекислого натри (рН р;еакционной смеси 10). Затем внос т при неремещивании 20,8 г (0,2 моль) 2,2-диаминодпэтилового эфира.156.6 g (1.2 mol) of chloromethlphosphinic acid is dissolved in 75 ml of distilled water, neutralized with 40% sodium hydroxide (96 g sodium hydroxide in 144 ml distilled water) and 47 g of anhydrous sodium carbonate (pH p; reaction mixture 10). Then, under dispensation, 20.8 g (0.2 mol) of 2,2-diamino ethyl ether are added.
Реакцию провод т в тех же услови х, как и при работе с днэтилентриамином (96 час нагревани при 108-110°С в токе азота). Свободную кислоту также выдел ют после удалени хлористого натри в сильно кислой среде путем осаждени метанолом и сущки в вакууме до посто нного веса. Получают 67 г тетраметилфосфиновой кислоты 2,2-диамииодиэтилового эфира, что составл ет 70% от те .оретического, счита на исходный амин.The reaction is carried out under the same conditions as in the operation with dethylenetriamine (96 hours of heating at 108-110 ° C in a stream of nitrogen). The free acid is also recovered after removal of sodium chloride in a strongly acidic medium by precipitation with methanol and in a vacuum to constant weight. 67 g of tetramethylphosphinic acid 2,2-diamiodioethylether are obtained, representing 70% of the theoretical, based on the starting amine.
Найдено, %: С 20,5; Н 5,1; N 5,84; Р 25,85. Вычислено, %: С 20,00; Н 5,03; N 5,83; Р 25,8.Found,%: C 20.5; H 5.1; N 5.84; R 25.85. Calculated,%: C 20.00; H 5.03; N 5.83; R 25.8.
Предмет изобретени Subject invention
Claims (2)
Publications (1)
| Publication Number | Publication Date |
|---|---|
| SU213865A1 true SU213865A1 (en) |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4931189A (en) * | 1988-11-02 | 1990-06-05 | Petrolite Corporation | Methods for inhibition of scale in high brine environments |
| US5112496A (en) * | 1988-11-02 | 1992-05-12 | Petrolite Corporation | Methods for inhibition of scale in high brine environments |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4931189A (en) * | 1988-11-02 | 1990-06-05 | Petrolite Corporation | Methods for inhibition of scale in high brine environments |
| US5112496A (en) * | 1988-11-02 | 1992-05-12 | Petrolite Corporation | Methods for inhibition of scale in high brine environments |
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