SU606860A1 - Method of preparing dichloranhydride of 1-chlor-2-diethylaminovinylphosphonic acid - Google Patents
Method of preparing dichloranhydride of 1-chlor-2-diethylaminovinylphosphonic acidInfo
- Publication number
- SU606860A1 SU606860A1 SU772446898A SU2446898A SU606860A1 SU 606860 A1 SU606860 A1 SU 606860A1 SU 772446898 A SU772446898 A SU 772446898A SU 2446898 A SU2446898 A SU 2446898A SU 606860 A1 SU606860 A1 SU 606860A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- diethylaminovinylphosphonic
- dichloranhydride
- chlor
- preparing
- acid
- Prior art date
Links
Description
В спектре, ЯМР промежуточного продукта присутствуют сигналы -219 м.д. (PCh), 4-298 м.д. (РС1 ), а также -75,4 м.д. и 67,2 м.д. Последние сигналы относитс к оргаии.чтри .члорфосфониевому катиону, по-видимому, к Ц11С- и г/ анс-фор.ме.In the spectrum, the NMR of the intermediate product signals are -219 ppm. (PCh), 4-298 ppm (PC1), as well as -75.4 ppm. and 67.2 ppm. The latter signals relate to the org. Thr. Chlorophosphonium cation, apparently to the C 11 C - and g / ans-form.
Пример. К раствору 41,7 г (0,2 мол ) PCL.s в 400 мл хлороформа при комнатной температуре добавл ют 27 г (0,27 мол ) триэтиламина в 50 мл хлороформа. Выдел етс осадок, который к концу добавлени триэтиламина раствор етс . Раствор приобретает темно-красную окраску . Через 1 сут растворитель удал ют при комнатной температуре в вакууме, бурый осадок обрабатывают SOj и летучие продукты удал ют в вакууме. Дихлорангидрид 1-хлор-2-диэтил аминовинилфосфоиовой кислоты экстрагируют эфиром, в остатке остаетс сол нокислый триэтиламин . Эфир отгон ют, а продукт перегон ют в вакууме. Выход 2,1 г (12,7%). Светлокоричневые кристаллы. Т. кип. 125-130°С (0,03 мм рт. ст.). Т. пл. 52°С (из гептана).Example. To a solution of 41.7 g (0.2 mol) of PCL.s in 400 ml of chloroform at room temperature was added 27 g (0.27 mol) of triethylamine in 50 ml of chloroform. A precipitate is precipitated, which dissolves by the end of the addition of triethylamine. The solution becomes a dark red color. After 1 day, the solvent is removed at room temperature under vacuum, the brown precipitate is treated with SOj and the volatile products are removed under vacuum. The 1-chloro-2-diethyl aminovinyl phosphonic acid dichloride is extracted with ether, and the residue remains hydrochloric triethylamine. The ether is distilled off and the product is distilled under vacuum. Yield 2.1 g (12.7%). Light brown crystals. T. Kip. 125-130 ° C (0.03 mm Hg. Art.). T. pl. 52 ° C (from heptane).
Вычислено, %: С 28,77; Н 4,42; Р 12,36; N 5,59; С1 42,46.Calculated,%: C, 28.77; H 4.42; R 12.36; N 5.59; C1 42.46.
СоНпСЬРО.SONPSIBRO.
Найдено, о/о: С 28,36; Н 4,69; Р 12,10; N 6,15; С1 41,05.Found, o / o: C 28.36; H 4.69; P 12.10; N 6.15; C1 41.05.
Claims (2)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| SU772446898A SU606860A1 (en) | 1977-01-24 | 1977-01-24 | Method of preparing dichloranhydride of 1-chlor-2-diethylaminovinylphosphonic acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| SU772446898A SU606860A1 (en) | 1977-01-24 | 1977-01-24 | Method of preparing dichloranhydride of 1-chlor-2-diethylaminovinylphosphonic acid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| SU606860A1 true SU606860A1 (en) | 1978-05-15 |
Family
ID=20693355
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| SU772446898A SU606860A1 (en) | 1977-01-24 | 1977-01-24 | Method of preparing dichloranhydride of 1-chlor-2-diethylaminovinylphosphonic acid |
Country Status (1)
| Country | Link |
|---|---|
| SU (1) | SU606860A1 (en) |
-
1977
- 1977-01-24 SU SU772446898A patent/SU606860A1/en active
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