SU514814A1 - The method of obtaining alkaline salts of p-tolylthiosulfonic - Google Patents
The method of obtaining alkaline salts of p-tolylthiosulfonicInfo
- Publication number
- SU514814A1 SU514814A1 SU2054273A SU2054273A SU514814A1 SU 514814 A1 SU514814 A1 SU 514814A1 SU 2054273 A SU2054273 A SU 2054273A SU 2054273 A SU2054273 A SU 2054273A SU 514814 A1 SU514814 A1 SU 514814A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- acid
- tolylthiosulfonic
- salt
- alkaline salts
- mol
- Prior art date
Links
- 238000000034 method Methods 0.000 title claims description 8
- 159000000011 group IA salts Chemical class 0.000 title claims description 5
- 239000002253 acid Substances 0.000 claims description 10
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 6
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 6
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- 159000000000 sodium salts Chemical class 0.000 claims description 3
- KEQGZUUPPQEDPF-UHFFFAOYSA-N 1,3-dichloro-5,5-dimethylimidazolidine-2,4-dione Chemical compound CC1(C)N(Cl)C(=O)N(Cl)C1=O KEQGZUUPPQEDPF-UHFFFAOYSA-N 0.000 claims description 2
- XTHPWXDJESJLNJ-UHFFFAOYSA-N chlorosulfonic acid Substances OS(Cl)(=O)=O XTHPWXDJESJLNJ-UHFFFAOYSA-N 0.000 claims description 2
- 239000012454 non-polar solvent Substances 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 claims description 2
- 239000011541 reaction mixture Substances 0.000 claims description 2
- UCGFRIAOVLXVKL-UHFFFAOYSA-N benzylthiourea Chemical class NC(=S)NCC1=CC=CC=C1 UCGFRIAOVLXVKL-UHFFFAOYSA-N 0.000 claims 2
- 239000011734 sodium Substances 0.000 claims 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims 1
- 239000007864 aqueous solution Substances 0.000 claims 1
- SSBBQNOCGGHKJQ-UHFFFAOYSA-N hydroxy-(4-methylphenyl)-oxo-sulfanylidene-$l^{6}-sulfane Chemical compound CC1=CC=C(S(S)(=O)=O)C=C1 SSBBQNOCGGHKJQ-UHFFFAOYSA-N 0.000 claims 1
- 238000002844 melting Methods 0.000 claims 1
- 230000008018 melting Effects 0.000 claims 1
- 239000002244 precipitate Substances 0.000 claims 1
- 239000000047 product Substances 0.000 claims 1
- 229920006395 saturated elastomer Polymers 0.000 claims 1
- QRQVSULAUMCUKL-UHFFFAOYSA-M sodium;1-methyl-4-sulfonatosulfanylbenzene Chemical compound [Na+].CC1=CC=C(SS([O-])(=O)=O)C=C1 QRQVSULAUMCUKL-UHFFFAOYSA-M 0.000 claims 1
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 2
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 description 2
- JMKQVEZUTYCVKD-UHFFFAOYSA-N 2h-pyridine-1-sulfonic acid Chemical compound OS(=O)(=O)N1CC=CC=C1 JMKQVEZUTYCVKD-UHFFFAOYSA-N 0.000 description 1
- WLHCBQAPPJAULW-UHFFFAOYSA-N 4-methylbenzenethiol Chemical compound CC1=CC=C(S)C=C1 WLHCBQAPPJAULW-UHFFFAOYSA-N 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 150000001447 alkali salts Chemical class 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- YBBRCQOCSYXUOC-UHFFFAOYSA-N sulfuryl dichloride Chemical compound ClS(Cl)(=O)=O YBBRCQOCSYXUOC-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Pyridine Compounds (AREA)
Description
(54) СПОСОБ ПОЛУЧЕНИЯ ЩЕЛОЧНЫХ СОЛЕЙ f ТОЛИЛТИОСУЛЬФОКИСЛОТЪ(54) METHOD OF OBTAINING ALKALINE SALTS f TOLYLTIOSULPHOXYL ACID
Изобретение относитс к новому способу пог1учени не описанных в литературе щелочных солей ft -толилтиосульфокислоты, ко торые могут найти применение в качестве биологически активных веществ.The invention relates to a new method for preparing alkali salts of ft-tolylthiosulfonic acid, which are not described in the literature, and which can be used as biologically active substances.
Известен способ получени пиридикиевой соли Л толилтиосульфокислоты. заключа ющи14с в том, что -тиокрезол подвергают взаимодействию с N -сульфопириди- ном в кип щем четыреххлористом углероде, A known method for producing the pyridic salt L of tolylthiosulfonic acid. implying that β-thiocresol is reacted with N-sulfopyridine in boiling carbon tetrachloride,
Однако в литературе отсутствуют сведе ни о способе получени щелочных солей П. -толилтиосульфокислоты, обладающих ценными свойствами.However, in the literature there is no information on the method of obtaining alkaline salts of P.-tolylthiosulfonic acid, which has valuable properties.
Предлагают способ получени щелочных солей fl -толилтиосульфокислоты, заклю чающийс в том, что Н -тиокрезол под вергают взаимодействию с хлорсульфоновой кислотой в среде непол рного растворител при 5-15-С. Процесс предпочтительно провод т в эфире, бензоле или хлористом мети лене.A method for the preparation of alkaline salts of fl-tolylthiosulfonic acid is proposed, in that H-thiocresol is reacted with chlorosulfonic acid in a medium of nonpolar solvent at 5-15 ° C. The process is preferably carried out in ether, benzene or methylene chloride.
Выход целевого продукта 97%. ft -Толилтиосульфокислота идентифицирована с помощью бензилтиурониевой соли, The yield of the target product is 97%. ft -Tolylthiosulfonic acid identified by the benzylthiuronic salt,
котора получена при реакции натриевой соли h -толллтиосульфокислоты с бензил- тиуро нийхлоридом.which is obtained by the reaction of sodium salt of h-tlthiosulfonic acid with benzylthiurochloride.
Бе зюттиурониева сохгь п-толилтиосу.пьфокислоты - бесцветный кристаллический продукт с т. пл. 183 С.Bezuttiuroneceae soch p-tolylthios. The acid is a colorless crystalline product with so pl. 183 C.
Пример 1. В колбе, снабженной механической мешагкой и делительной ворокой , раствор ют 1,24 г (0,01 моль) п-тиокрезола в 50 мл растворител , охлаждают до 15 С, прикапывают 0,65 мл (0,01 моль) хлорсульфоновой кислоты в 1О мл соответствующего растворител . Реакционную смесь перемешивают в течени 30 мин при комнатной температуре. Затем растворитель удал ют в вакууме. Остаток выливают в раствор 0,8 г (0,02 моль) едкого натра, в 30 мл этанола. Выпавший осадок отфильтровывают, промывают спиртом , эфиром.Example 1. 1.24 g (0.01 mol) of p-thiocresol is dissolved in 50 ml of solvent in a flask equipped with a mechanical bag and a separating head, cooled to 15 ° C, 0.65 ml (0.01 mol) of chlorosulfone is added dropwise. acid in 1O ml of an appropriate solvent. The reaction mixture is stirred for 30 minutes at room temperature. The solvent is then removed in vacuo. The residue is poured into a solution of 0.8 g (0.02 mol) of sodium hydroxide in 30 ml of ethanol. The precipitation is filtered off, washed with alcohol, ether.
Claims (2)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| SU2054273A SU514814A1 (en) | 1974-08-22 | 1974-08-22 | The method of obtaining alkaline salts of p-tolylthiosulfonic |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| SU2054273A SU514814A1 (en) | 1974-08-22 | 1974-08-22 | The method of obtaining alkaline salts of p-tolylthiosulfonic |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| SU514814A1 true SU514814A1 (en) | 1976-05-25 |
Family
ID=20594304
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| SU2054273A SU514814A1 (en) | 1974-08-22 | 1974-08-22 | The method of obtaining alkaline salts of p-tolylthiosulfonic |
Country Status (1)
| Country | Link |
|---|---|
| SU (1) | SU514814A1 (en) |
-
1974
- 1974-08-22 SU SU2054273A patent/SU514814A1/en active
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