SU178803A1 - METHOD OF OBTAINING N- OR N, N'-PILZAILS OF CHARACTERISTIC FORMAMIDINSULPHINE ACIDS - Google Patents
METHOD OF OBTAINING N- OR N, N'-PILZAILS OF CHARACTERISTIC FORMAMIDINSULPHINE ACIDSInfo
- Publication number
- SU178803A1 SU178803A1 SU939685A SU939685A SU178803A1 SU 178803 A1 SU178803 A1 SU 178803A1 SU 939685 A SU939685 A SU 939685A SU 939685 A SU939685 A SU 939685A SU 178803 A1 SU178803 A1 SU 178803A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- acids
- obtaining
- pilzails
- formamidinsulphine
- characteristic
- Prior art date
Links
- 239000002253 acid Substances 0.000 title description 5
- 150000007513 acids Chemical class 0.000 title description 3
- MHAJPDPJQMAIIY-UHFFFAOYSA-N hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 6
- 239000002244 precipitate Substances 0.000 description 2
- KEAYESYHFKHZAL-UHFFFAOYSA-N sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- YKSCOZXTXACAIX-UHFFFAOYSA-N N'-phenylmethanimidamide Chemical compound N=CNC1=CC=CC=C1 YKSCOZXTXACAIX-UHFFFAOYSA-N 0.000 description 1
- FULZLIGZKMKICU-UHFFFAOYSA-N Phenylthiocarbamide Chemical compound NC(=S)NC1=CC=CC=C1 FULZLIGZKMKICU-UHFFFAOYSA-N 0.000 description 1
- UMGDCJDMYOKAJW-UHFFFAOYSA-N Thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 1
- 235000013601 eggs Nutrition 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- -1 formamidine sulfonic acids Chemical class 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 description 1
- 230000003287 optical Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-N sulfonic acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Description
Предложеи сиособ иолучеии N- или N,Nарилзамеидеииых формамидинсульфииовых кислот, состо щий в том, что N- или N,Nарилзамещеииую тиомочевииу обрабатывают перекисью водорода ири температуре от О до -f-15°C в присутст.вии молибденовокислого иатри в среде растворител .Suggest siosob iolucheii N- or N, Narilzameideiiyh formamidinsulfiiovyh acids, consisting in the fact that the N- or N, Narilzamescheiiuyu tiomocheviiu treated with hydrogen peroxide iri a temperature of from O to -f-15 ° C in prisutst.vii iatri molybdate in a solvent.
Пример 1. Получение N-ф е н и лф о р м а м и д и и с у л ь ф и и о в о и кислот ы. В двухгорлую колбу, снабженную мешалкой, термометром и капельиой воронкой, загружают 2 г N-фенилтиомочевииы, 0,005 г молибдеиовокислого иатри и приливают 10 мл воды . Смесь охлаждают до О-5°С и добавл ют по капл м 3 мл (31,2%) перекиси водорода, поддержива ту же температуру, после чего массу при размешивании выдерживают в течение 1 час при температуре от О до 5°С. Белый осадок отфильтровывают и высушивают при температуре . Получают 1 г N-фенилформамидинсульфииовой кислоты, что составл ет 41,4% от теоретического, счита на Nфеиилтиомочевииу .Example 1. Preparation of N-fen and lf o rm and m and d and and with l and f and and o about and acids. In a two-neck flask equipped with a stirrer, a thermometer, and a dropping funnel, 2 g of N-phenylthiourea, 0.005 g of molybdeioic acid and sodium are added and 10 ml of water are added. The mixture is cooled to -5 ° C and 3 ml (31.2%) of hydrogen peroxide is added dropwise, maintaining the same temperature, after which the mass is kept under stirring for 1 hour at a temperature from 0 to 5 ° C. The white precipitate is filtered off and dried at a temperature. 1 g of N-phenylformamidine sulfonic acid is obtained, which constitutes 41.4% of the theoretical value, based on Ntheiylthiourea.
Вычислено, %: С 45,60; II 4,35; N 15,20.Calculated,%: C 45.60; II 4.35; N 15.20.
CynsNaOoS.CynsNaOoS.
лоты, в трехгорлую колбу, снабженную мешалкой , термомегром и капельиой воронкой, загружают 5 г N.X-дифеннлтномочевииы и приливают 80 мл диоксаиа. Раствор охлаждают лЮ 15°С н добавл ют 0,025 г молибдеиовокислого иатри . При эиергичиом размешинанни при температуре 15°С по капл м приливают 6 мл (28,2%) иерекнси водорода. По окончании прибавлени температуру массы снижают до 5°С, при этом выпадает осадок, lots, in a three-necked flask equipped with a stirrer, a thermo-megrome and a dropping funnel, are charged with 5 g of N.X.-difennlt-powers and 80 ml of dioxa are poured. The solution is cooled at a temperature of 15 ° C. 0.025 g of molybdium acid and sodium are added. When the egg splash is placed at a temperature of 15 ° C, 6 ml (28.2%) of hydrogen is added dropwise. At the end of the addition, the temperature of the mass is reduced to 5 ° C, and a precipitate appears,
0 который отфильтровывают п суншт при температуре 60°С. Получают 4 г К,М-дифеи11лформамидинсульфиновой кислоты, что составл ет 64,5% от теоретического, счита иа Х ,Х-дифенилтиомочевииу .Which is filtered n sunsht at a temperature of 60 ° C. 4 g of K, M-dipheyl 11 -formamidinesulfinic acid is obtained, which is 64.5% of the theoretical value, including X, X-diphenylthiourea.
5five
Вычислено, %: С 52,70; П 5,40; N 9,46. CKsH7N.O.,S 2П.0.Calculated,%: C, 52.70; P 5.40; N 9.46. CKsH7N.O., S 2П.0.
Найдеио, %: С 52,26; 52,60; Н 4,86; 5,08; N9,05; 9,13.Naidio,%: C, 52.26; 52.60; H 4.86; 5.08; N9.05; 9.13.
Предмет изобретени Subject invention
Способ получени N- или М,Ы-арилзамещеиных формамидинсульфиновых кислот, огличающийс тем, что N- или М,Ы-арилзамощеииую тиомочевину иодвергают взаимодейсг5 пию с перекисью водорода при температуре от О до - 15°С; в присутствш молибдеиовокислого иатри в среде растворител с последуюии1М выделением готового продукта фпльтрапией.The method of obtaining N- or M, N-aryl-substituted formamidine sulfonic acids, stating that N- or M, N-aryl-containing thiourea and react with hydrogen peroxide at a temperature from 0 to –15 ° C; in the presence of molybdium iatrium in a solvent medium followed by the release of the final product by optical trap.
Publications (1)
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SU178803A1 true SU178803A1 (en) |
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4656291A (en) * | 1985-03-15 | 1987-04-07 | Mcneilab, Inc. | Process for producing amidine sulfonic acids |
US4656270A (en) * | 1985-03-15 | 1987-04-07 | Mcneilab, Inc. | Process for producing guanidines such as linogliride |
US4781866A (en) * | 1985-03-15 | 1988-11-01 | Mcneilab, Inc. | Process for producing amidine sulfonic acid intermediates for guanidines |
US4851094A (en) * | 1985-03-15 | 1989-07-25 | Mcneilab, Inc. | Process for producing amidine sulfonic acid intermediates for guanidines |
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4656291A (en) * | 1985-03-15 | 1987-04-07 | Mcneilab, Inc. | Process for producing amidine sulfonic acids |
US4656270A (en) * | 1985-03-15 | 1987-04-07 | Mcneilab, Inc. | Process for producing guanidines such as linogliride |
US4781866A (en) * | 1985-03-15 | 1988-11-01 | Mcneilab, Inc. | Process for producing amidine sulfonic acid intermediates for guanidines |
US4851094A (en) * | 1985-03-15 | 1989-07-25 | Mcneilab, Inc. | Process for producing amidine sulfonic acid intermediates for guanidines |
EP0248586A2 (en) * | 1986-05-28 | 1987-12-09 | McNeilab, Inc. | Process for producing amidine sulfonic acid intermediates for guanidines |
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