SU527421A1 - The method of obtaining oxamic acid arenesulfonylamides - Google Patents

The method of obtaining oxamic acid arenesulfonylamides

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Publication number
SU527421A1
SU527421A1 SU2110007A SU2110007A SU527421A1 SU 527421 A1 SU527421 A1 SU 527421A1 SU 2110007 A SU2110007 A SU 2110007A SU 2110007 A SU2110007 A SU 2110007A SU 527421 A1 SU527421 A1 SU 527421A1
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SU
USSR - Soviet Union
Prior art keywords
aliphatic amine
obtaining
oxamic acid
arenesulfonylamides
acid
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Application number
SU2110007A
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Russian (ru)
Inventor
Павел Алексеевич Петюнин
Иван Прокофьевич Банный
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Харьковский государственный фармацевтический институт
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Priority to SU2110007A priority Critical patent/SU527421A1/en
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Publication of SU527421A1 publication Critical patent/SU527421A1/en

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(54) СПОСОБ ПОЛУЧЕНИЯ АРЕНСУЛЬФОНИЛАМИДОВ ОКСАМИНОВЫХ КИСЛОТ(54) METHOD FOR OBTAINING ARENSULPHONYLAMIDES OF OXAMINE ACIDS

амина, как только среда перестанет быть щелочной, большую часть метанола отгон ют, раствор ют остаток в 5-кратном количестве воды, фильтруют, подкисл ют фильтрат сол ной кислотой (1:1) до , фильтруют, кристаллизуют осадок и получают 4,52 г продукта.amine, once the medium is no longer alkaline, most of the methanol is distilled off, the residue is dissolved in 5 times the amount of water, filtered, the filtrate is acidified with hydrochloric acid (1: 1) to filtered, the precipitate crystallizes and 4.52 g are obtained product.

Пример 2. Изобутиламид п-толуолсульфонилоксаминовой кислоты.Example 2. P-toluenesulfonyloxamic acid isobutylamide.

В тех же услови х, что и в примере 1, после нагревани  до исчезновени  малинового окрашивани  большую часть метанола отгон ют, раствор ют остаток в 5-кратном количестве воды, фильтруют , подкисл ют фильтрат сол ной кислотой (1:1) до рН 5, отфильтровьшают осадок, кристаллизуют и получают 3,4 г этилового эфира п-толуолсульфонилоксаминовой кислоты.Under the same conditions as in Example 1, after heating until the crimson color disappears, most of the methanol is distilled off, the residue is dissolved in 5-fold amount of water, filtered, the filtrate is acidified with hydrochloric acid (1: 1) to pH 5 The precipitate is filtered off and crystallized to obtain 3.4 g of p-toluenesulfonyloxamic acid ethyl ester.

К раствору 3,4 г полученного вещества в 10 мл этанола прибавл ют 1,83 г изобутиламина, как только среда перестанет быть щелочной, большую часть этанола отгон ют, поступают, как в примере 1, и получают 3,04 г целевого продукта.To a solution of 3.4 g of the obtained substance in 10 ml of ethanol was added 1.83 g of isobutylamine, as soon as the medium ceased to be alkaline, most of the ethanol was distilled off, proceeded as in Example 1, and 3.04 g of the desired product are obtained.

В примерах 1 и 2 выход целевого продукта дан в пересчете на вз тый в реакцию п-толуолсульфамид .In Examples 1 and 2, the yield of the desired product is given in terms of the p-toluenesulfamide reacted.

СНзЦиклогексилCHS Cyclohexyl

СНз(СНз)2СНСН2CH3 (CH3) 2CHCH2

СНзНОСНз СНзSNSNOSNZ SNZ

NH2ЦиклогексилNH2 Cyclohexyl

МНСООСНз НОСНгСНзMNESOPHOSHSS

Claims (1)

Формула изобретени Invention Formula Способ получени  аренсульфониламидов оксаминовых кислот путем взаимодействи  аренсульфамида с диэтилоксалатом в присутствии метилата натри  с последующей обработкой алифатическим амином и выделением целевого продукта при подкислении, отличающийс  тем, что, с целью упрощени  технологии процесса и увеличеш{  выхода целевого продукта, реакционную массу.A process for the preparation of oxamic acid aresulfonyl amides by reacting arensulfonamide with diethyl oxalate in the presence of sodium methoxide followed by treatment with aliphatic amine and isolating the target product during acidification, characterized in that, in order to simplify the process technology and increase the yield of the target product, the reaction mass. 58,2 51,4 61,2 50,0 44,958.2 51.4 61.2 50.0 44.9 полученную путем взаимодействи  аренсульфамида с диэтилоксалатом, непосредственно подвергают обработке алифатическим амином при мол рном соотношении между аренсульфамидом и алифатическим амином, равном 1 - 1,1:1.obtained by reacting arensulfonamide with diethyloxalate, directly treated with an aliphatic amine at a molar ratio between isrensulfamide and an aliphatic amine of 1-1.1: 1. Источники информации, прин тые во внимание при экспертизе:Sources of information taken into account in the examination: I. П. А. Петюнин и др., Аренсульфониламиды оксаминовьк кислот, ЖОРХ, 3, 130, 1967.I.P.A. Petyunin et al., Arensulfonylamides of oxamino acid, JORH, 3, 130, 1967.
SU2110007A 1975-02-28 1975-02-28 The method of obtaining oxamic acid arenesulfonylamides SU527421A1 (en)

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