SU66327A1 - The method of obtaining the disodium salt of 4,4'-diglycyldiphenyl-sulfone - Google Patents
The method of obtaining the disodium salt of 4,4'-diglycyldiphenyl-sulfoneInfo
- Publication number
- SU66327A1 SU66327A1 SU4960A SU336695A SU66327A1 SU 66327 A1 SU66327 A1 SU 66327A1 SU 4960 A SU4960 A SU 4960A SU 336695 A SU336695 A SU 336695A SU 66327 A1 SU66327 A1 SU 66327A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- solution
- diglycyldiphenyl
- sulfone
- obtaining
- disodium salt
- Prior art date
Links
- 238000000034 method Methods 0.000 title description 3
- QXNVGIXVLWOKEQ-UHFFFAOYSA-N Disodium Chemical class [Na][Na] QXNVGIXVLWOKEQ-UHFFFAOYSA-N 0.000 title description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 235000011121 sodium hydroxide Nutrition 0.000 description 2
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 1
- 239000005751 Copper oxide Substances 0.000 description 1
- MQJKPEGWNLWLTK-UHFFFAOYSA-N Dapsone Chemical compound C1=CC(N)=CC=C1S(=O)(=O)C1=CC=C(N)C=C1 MQJKPEGWNLWLTK-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- ZGUNAGUHMKGQNY-ZETCQYMHSA-N L-alpha-phenylglycine zwitterion Chemical compound OC(=O)[C@@H](N)C1=CC=CC=C1 ZGUNAGUHMKGQNY-ZETCQYMHSA-N 0.000 description 1
- 150000004982 aromatic amines Chemical class 0.000 description 1
- 239000003518 caustics Substances 0.000 description 1
- 230000000973 chemotherapeutic effect Effects 0.000 description 1
- FOCAUTSVDIKZOP-UHFFFAOYSA-N chloroacetic acid Chemical compound OC(=O)CCl FOCAUTSVDIKZOP-UHFFFAOYSA-N 0.000 description 1
- 229940106681 chloroacetic acid Drugs 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 150000001879 copper Chemical class 0.000 description 1
- 229910000431 copper oxide Inorganic materials 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- KDYFGRWQOYBRFD-UHFFFAOYSA-L succinate(2-) Chemical compound [O-]C(=O)CCC([O-])=O KDYFGRWQOYBRFD-UHFFFAOYSA-L 0.000 description 1
Landscapes
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Cosmetics (AREA)
Description
Получение глицилпроиэводного диаминодифенилсульфона протекает не так гладко, как это имеет место в случа|е простых аромафических аминюв, вследствие чего .применение способов, описанных дл получени фенилглицина, не шрвводит в данHJOM случае к полю жительным реsyijibTaTaiM .The preparation of glycylprodiamine diaminodiphenylsulfone does not proceed as smoothly as it does in the case of simple aromatic amines, as a result of which the use of the methods described for the preparation of phenylglycine does not lead in this HJOM case to positive resijijTaTaiM.
Автором pai3ipiai6oTaH способ полу4ieiHiHH йатриев скй соли 4,4-диглицилдифенилсульфо а из хлоруксуснокислого натри и 4,4-диаминодифенилсульфона , характеризуюш,ийс тем, что реакци проводитс в водноспиртовой сре1де при длительном .нагревании реакционной смеои. Конечный продукт выдел етс спиртом в В«де натриевой соли. Очистка вещества от небольшой примеси хлористого натри производитс переводом его в дню растворимую медную солЬ с послгдующиа (разложеиювм ее вычиоленным количеством О01ДЫ.The author pai3ipiai6oTaH method polu4ieiHiHH yatra salt sky and 4,4-diglitsildifenilsulfo hloruksusnokislogo of sodium 4,4-diaminodiphenylsulfone, harakterizuyush, iys in that the reaction is carried out in hydroalcoholic sre1de prolonged reaction .nagrevanii smeoi. The final product is isolated with alcohol in a "de sodium salt". Purification of a substance from a small admixture of sodium chloride is carried out by transferring it into a day of soluble copper salt with the next (decomposing it with the required amount of O1DY.
Соединение вл етс химиотерапевтичбсюкм оредотвоМ.The compound is a chemotherapeutic chemoprotein.
Пример. 56,7 г (0,6 мол ) хлоруксусной кислоты точно нейтрализуют 40-п роцент;нъ1м раствором едкого йатри И смешивают с 125 мл воды и ЮО мл 96-1процент1ного спирта. К полученному раствору прибавл ют 62 г (0,25 1мол ) 4,4-диами:Н10Дифе ИлгульфоНа и смесь кип т т 10-/2 часов до ПОЛНОЙ растворимости пробы в разбавлен)ном едком натре. Раствор обрабатывают едким натром до слабощелочной реакции на лаюмус, нагревают еще 3 часа, разбавл ют (двойнъш объеMOiMi Воды н фильтруют. Фильтрат упаривают на вод ной баие до консистенции сирапа и разба1вл ют спиртом. Осадок отфильтровывают, промывают спиртом и высушивают. Выход 83,2 г, или 81,7%.Example. 56.7 g (0.6 mol) of chloroacetic acid exactly neutralizes the 40% concentration; 1m solution of caustic Yatry I is mixed with 125 ml of water and 10 ml of 96-1 percent alcohol. 62 g (0.25 1 mol) of 4,4-diami: H10 Dif IlgulfoNa was added to the solution obtained and the mixture was boiled for 10- / 2 hours until the sample was FULLY soluble in diluted sodium hydroxide solution. The solution is treated with caustic soda to a weakly alkaline reaction to Laumus, heated for another 3 hours, diluted (double volume of MOiMi Water n is filtered. The filtrate is evaporated on water to a sirap consistency and diluted with alcohol. The precipitate is filtered, washed with alcohol and dried. Output 83.2 g, or 81.7%.
Дл очи1гтк)и водньш раствор полученной динатрие&ой соли 4,4диглицилдифенилсульфона обрабатывают при нагревании небольШим избыткол раствора .медного купо.роса, выделившуюс , трудно растворимую медную оань отсасыВают , промывают водой, разлагают вычисленным .количест1вом раствора соды при кип чении, раствор отфильт .ровьивйют от окиси меди, фильтрат упарнвают и обрабатывают сииртбМ;№ 66327 - 2-For a solution) and a water solution of the obtained disodium & 4,4 diglycyldiphenylsulfone salt is treated by heating with a small excess of copper cupro solution, separated, difficultly soluble copper oan is sucked off, washed with water, decomposed with a solution of solution and washed with water, decomposed by dissolving copper solution, washed with water, dispersed with a solution of solution and washed with water; levitate from copper oxide, the filtrate is evaporated and treated with silicone; № 66327 - 2-
П ip е д:1ч е т и 3 о б р е т е и и в. «Одйа-Опйртоиой ореде с хлорук„ .,суюнокислым iHiaiipHeM. затем омесьP ip e d: 1 t e t and 3 o b e t e i u c. “Odya-Opyrtoyoy oreda with Chloruk„., Succinate iHiaiipHeM. then knead
Способ пйлученй дни атриев ои г iThe way you want the days of the atrei oi g i
ооли 4,4-диглиц.илд1И,фанижульфова,ВДДЩелачишют и из упаренногоooli 4,4-diglits.ildiI, fanizhulfova, VDDchelachuyut and from one stripped off
отличающийс тем, что 4,4-р1а1створа продукт высаживают придиамййодифениисульфой нагр ваютбавлением спирта.characterized in that 4,4-p1a1 of the solution, the product is precipitated by pridiamaydiphenisisulfa and is heated by the addition of alcohol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| SU4960A SU66327A1 (en) | 1945-02-13 | 1945-02-13 | The method of obtaining the disodium salt of 4,4'-diglycyldiphenyl-sulfone |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| SU4960A SU66327A1 (en) | 1945-02-13 | 1945-02-13 | The method of obtaining the disodium salt of 4,4'-diglycyldiphenyl-sulfone |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| SU66327A1 true SU66327A1 (en) | 1945-11-30 |
Family
ID=51358271
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| SU4960A SU66327A1 (en) | 1945-02-13 | 1945-02-13 | The method of obtaining the disodium salt of 4,4'-diglycyldiphenyl-sulfone |
Country Status (1)
| Country | Link |
|---|---|
| SU (1) | SU66327A1 (en) |
-
1945
- 1945-02-13 SU SU4960A patent/SU66327A1/en active
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