SU367095A1 - ALL-UNION I - Google Patents
ALL-UNION IInfo
- Publication number
- SU367095A1 SU367095A1 SU1641007A SU1641007A SU367095A1 SU 367095 A1 SU367095 A1 SU 367095A1 SU 1641007 A SU1641007 A SU 1641007A SU 1641007 A SU1641007 A SU 1641007A SU 367095 A1 SU367095 A1 SU 367095A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- union
- mol
- acetic acid
- preparation
- sodium thiosulfate
- Prior art date
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- Indole Compounds (AREA)
Description
1one
Изобретение относитс к области получени соединений, которые могут найти применение в фармацевтической промыпдленности.The invention relates to the field of the preparation of compounds which can be used in the pharmaceutical industry.
Использование известного метода восстановлени нитросоедннений хлористым оловом привело к получению новых соединений индольного р да, р-индолил-3-р-.меркаптоалкиламинов , обладающих .физиологической активностью .The use of the known method for the reduction of nitroassays with tin chloride resulted in the preparation of new compounds of the indole series, p-indolyl-3-p-mercaptoalkylamines, which have physiological activity.
Предлагаемый способ получени солей Риндолил-3-р-меркаптоалкиламинов заключаетс в том, что меркаптонитросоединение подвергают восстановлению сол ми металлов переменной валентности, например раствором безводного хлористого олова в лед ной уксусной кислоте. Все дальнейшие обработки также провод тс в кислой среде, что дает возможность непосредственно получать соль меркаптоамина , исключа стадию выделени нестойкого основани . Реакцию провод т при температуре от О до 15°С, предпочтительно при 3-5°С. Целевой продукт выдел ют известными методами.The proposed method for the preparation of the salts of Rindolyl-3-p-mercaptoalkylamines is that the mercapton-nitro compound is subjected to reduction with variable valence metal salts, for example, with an anhydrous tin chloride solution in glacial acetic acid. All further treatments are also carried out in an acidic medium, which makes it possible to directly obtain the mercaptoamine salt, excluding the step of isolating the unstable base. The reaction is carried out at a temperature from 0 to 15 ° C, preferably at 3-5 ° C. The desired product is isolated by known methods.
Использу метод присоединени тиосульфата натри к эфирам акриловых кислот, получают исходные меркаптонитросоединени взаимодействием тиосульфата натри с 1-ацетил3-нитровинилиндолом . Using the method of adding sodium thiosulfate to acrylic acid esters, the starting mercaptonitro compounds are obtained by reacting sodium thiosulfate with 1-acetyl3-nitrovinylindole.
Пример 1. Гор чий раствор 11,5 г (0,05 моль) 1-ацетил-З-нитровинилиндола в 210 мл лед ной уксусной кислоты приливаютExample 1. A hot solution of 11.5 g (0.05 mol) of 1-acetyl-3-nitrovinylindole in 210 ml of glacial acetic acid is poured
порци ми к раствору 74,4 г (0,3 моль) тиосульфата натри в 280 мл воды таким образом , чтобы температура не поднималась выше 40°С. Нагревают 5 час при 40°С, отфильтровывают бесцветный осадок, промывают его водой, подкисленной уксусной кислотой. После высушивани на воздухе получают 11,8 г смеси I и П. Смесь подвергают дробной кристаллизации из хлороформа.in portions to a solution of 74.4 g (0.3 mol) of sodium thiosulfate in 280 ml of water so that the temperature does not rise above 40 ° C. Heated for 5 hours at 40 ° C, the colorless precipitate is filtered off, washed with water, acidified with acetic acid. After air drying, 11.8 g of a mixture of I and P. are obtained. The mixture is subjected to fractional crystallization from chloroform.
Получают 4,1 г (28%) бесцветных кристаллов (1-ацетил№ндолил-3)-2-Н1 троэт1)л дисульфида (I). Т.пл. 14ГС (лосле высушивани в вакууме над хлористым кальцием при 30°С).4.1 g (28%) of colorless crystals (1-acetyl-#indolyl-3) -2-H1 troeth1) of disulfide (I) are obtained. M.p. 14 ° C (vacuum drying over calcium chloride at 30 ° C).
Найдено, %: С 50,00; Н 4,00; N 9,32; S 11,08.Found,%: C 50.00; H 4.00; N 9.32; S 11.08.
C24H22N406S2C24H22N406S2
Вычислено, %: С 50,20; Н 3,86; N 9,55; S 10,91.Calculated,%: C 50.20; H 3.86; N 9.55; S 10.91.
VMaKc СЛ4-: 1694 (С О); 1560, 1334 (NO,); 773,762 (С-Н ароматика).VMaKc SL4-: 1694 (C O); 1560, 1334 (NO,); 773,762 (C-H aromatics).
Получают 2,3 г (17%) бесцветных кристаллов ди- 1- (1-ацетилиндолил-3) -2-нитроэтил трисульфида (II). Т. пл. 79°С.2.3 g (17%) of colorless crystals of di- 1- (1-acetylindolyl-3) -2-nitroethyl trisulfide (II) are obtained. T. pl. 79 ° C.
Найдено, %: С 51,28; Н 3,86; N 9,74; S 16,98.Found,%: C 51.28; H 3.86; N 9.74; S 16.98.
C,4H,oX.,SO.S,.C, 4H, oX., SO.S ,.
Вычислено, %: С 51,51; Н 3,96; S 17,18; N 9,86.Calculated,%: C 51.51; H 3.96; S 17.18; N 9.86.
VMnrr CM--: 1722 (С 0); 1552, 1326 (NC,); 740 (С-Н ароматика).VMnrr CM--: 1722 (C 0); 1552, 1326 (NC,); 740 (C – H aromatics).
Пример 2. 1,5 г (0,0027 моль) трисульфида II по примеру 1 прибавл ют при охлажExample 2. 1.5 g (0.0027 mol) of trisulfide II of example 1 is added during cooling
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
SU1641007A SU367095A1 (en) | 1971-04-02 | 1971-04-02 | ALL-UNION I |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
SU1641007A SU367095A1 (en) | 1971-04-02 | 1971-04-02 | ALL-UNION I |
Publications (1)
Publication Number | Publication Date |
---|---|
SU367095A1 true SU367095A1 (en) | 1973-01-23 |
Family
ID=20470813
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
SU1641007A SU367095A1 (en) | 1971-04-02 | 1971-04-02 | ALL-UNION I |
Country Status (1)
Country | Link |
---|---|
SU (1) | SU367095A1 (en) |
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1971
- 1971-04-02 SU SU1641007A patent/SU367095A1/en active
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