SU606860A1 - Method of preparing dichloranhydride of 1-chlor-2-diethylaminovinylphosphonic acid - Google Patents

Method of preparing dichloranhydride of 1-chlor-2-diethylaminovinylphosphonic acid

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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
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SU
USSR - Soviet Union
Prior art keywords
diethylaminovinylphosphonic
dichloranhydride
chlor
preparing
acid
Prior art date
Application number
SU772446898A
Other languages
Russian (ru)
Inventor
Галина Александровна Пенсионерова
Владимир Григорьевич Розинов
Владимир Иванович Глухих
Людмила Михайловна Сергиенко
Original Assignee
Иркутский государственный университет им. А.А.Жданова
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
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Application filed by Иркутский государственный университет им. А.А.Жданова filed Critical Иркутский государственный университет им. А.А.Жданова
Priority to SU772446898A priority Critical patent/SU606860A1/en
Application granted granted Critical
Publication of SU606860A1 publication Critical patent/SU606860A1/en

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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)

1.Авторское свидетельство СССР Л 476272, кл. С 07 F 9/40, 1973.1. Authors certificate of the USSR L 476272, cl. C 07 F 9/40, 1973. 2.I. R. Beattie, M.Webster. The Interaction of Phosphorus Pentachloride with Tertiary Amines , I. Chem Soc, 1961, c. 1730-1733.2.I. R. Beattie, M.Webster. The Interaction of Phosphorus Pentachloride with Tertiary Amines, I. Chem Soc, 1961, c. 1730-1733.
SU772446898A 1977-01-24 1977-01-24 Method of preparing dichloranhydride of 1-chlor-2-diethylaminovinylphosphonic acid SU606860A1 (en)

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

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Country Status (1)

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