PL366B1 - A method of obtaining arsenic-containing acids and their salts. - Google Patents
A method of obtaining arsenic-containing acids and their salts. Download PDFInfo
- Publication number
- PL366B1 PL366B1 PL366A PL36620A PL366B1 PL 366 B1 PL366 B1 PL 366B1 PL 366 A PL366 A PL 366A PL 36620 A PL36620 A PL 36620A PL 366 B1 PL366 B1 PL 366B1
- Authority
- PL
- Poland
- Prior art keywords
- arsenic
- salts
- acid
- containing acids
- obtaining
- Prior art date
Links
- 239000002253 acid Substances 0.000 title claims description 9
- 229910052785 arsenic Inorganic materials 0.000 title claims description 9
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 title claims description 9
- 150000003839 salts Chemical class 0.000 title claims description 5
- 150000007513 acids Chemical class 0.000 title claims description 3
- 238000000034 method Methods 0.000 title claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 4
- XNERWVPQCYSMLC-UHFFFAOYSA-N phenylpropiolic acid Chemical compound OC(=O)C#CC1=CC=CC=C1 XNERWVPQCYSMLC-UHFFFAOYSA-N 0.000 claims description 4
- 239000003513 alkali Substances 0.000 claims description 3
- OEYOHULQRFXULB-UHFFFAOYSA-N arsenic trichloride Chemical compound Cl[As](Cl)Cl OEYOHULQRFXULB-UHFFFAOYSA-N 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 239000011591 potassium Substances 0.000 description 4
- 229910052700 potassium Inorganic materials 0.000 description 4
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 229910052736 halogen Inorganic materials 0.000 description 2
- 239000003208 petroleum Substances 0.000 description 2
- 238000001953 recrystallisation Methods 0.000 description 2
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical group 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
- 230000002378 acidificating effect Effects 0.000 description 1
- JMBNQWNFNACVCB-UHFFFAOYSA-N arsenic tribromide Chemical compound Br[As](Br)Br JMBNQWNFNACVCB-UHFFFAOYSA-N 0.000 description 1
- 229940077468 arsenic tribromide Drugs 0.000 description 1
- GCPXMJHSNVMWNM-UHFFFAOYSA-N arsenous acid Chemical compound O[As](O)O GCPXMJHSNVMWNM-UHFFFAOYSA-N 0.000 description 1
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 1
- 229910052794 bromium Inorganic materials 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 125000004344 phenylpropyl group Chemical group 0.000 description 1
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Description
W patencie glównym niemieckim 257641 oraz patentach dodatkowych 268829, 271159 i 273219 opisano sposoby otrzymywania kwasów tluszczowych, zawierajacych arsen, oraz ich pochodnych, polegajace na tern, ze kwasy rzedu ace¬ tylenowego lub ich pochodne poddaje sie dzialaniu trójchlorowcowych pochod¬ nych arsenu lub tez mieszanin, wytwa¬ rzajacych te pochodne, wzglednie reagu¬ jacych jak one.Stwierdzono, ze mozna, w przeci¬ wienstwie do otrzymywanych ta droga produktów bezpostaciowych, otrzymac ladnie skrystalizowane ciala, jezeli pod¬ daje sie kwas fenylopropiolowy dziala¬ niu reakcyj, opisanych w.podanych pa¬ tentach. Tak otrzymana pochodna kwasu fenylopropiolowego z zawartoscia arsenu znamienna jest, prócz wlasciwosci kry¬ stalizowania, latwa podatnoscia do od¬ dzielenia chlorowca przy dzialaniu sla¬ bych alkalij, przyczem otrzymuje sie takze sole w krysztalach.Przyklad 1. 20 czesci wagowych kwasu fenylo¬ propiolowego podgrzewa sie w 50 cze¬ sciach wagowych trójchlorku arsenowego w ciagu 24 godzin do 100°. Z plynu reakcyjnego wydzielaja sie przy staniu lub dodaniu eteru krysztaly listkowe, które po odsaczeniu, plókaniu eterem i przekrystalizowaniu sa zupelnie bez¬ barwne i zawieraja mniej wiecej 14.5% chloru oraz okolo 16 % arsenu. Sa one nierozpuszczalne w wodzie, rozpuszczaja sie natomiast w goracym, acetonie, chlo¬ roformie i benzolu, trudniej w eterze.Jezeli rozpusci sie 15 czesci tego kwasu w 120 czesciach póltora raza nor-malnego lugu potasowego przy 0° i wpro¬ wadza w danym razie do przesaczonego plynu kwas weglowy, oddziela sie, jako papka krystaliczna, sól potasowa kwasna krystaliczna z zawartoscia wody. Po przekrystalizowaniu z 10-ciokrotnej ilosci goracej wody i po usunieciu wody kry- stalizacyjnej zawiera ona okolo \ 17% arsenu, rozpuszcza sie z * latwoscia w zimnych alkaljach lub weglanach alka¬ licznych, a przy podgrzaniu w nadmiarze alkalij na kapieli wodnej wydziela kwas arsenawy.Przyklad 2. 50 czesci wagowych kwasu fenylo- propiolowego podgrzewa sie w 200 cze¬ sciach trójbromku arsenowego w ciagu 20 godzin do 100°. Mase reakcyjna roz¬ puszcza sie w malej ilosci eteru i do¬ daje niewielka ilosc eteru naftowego.Wydzielaja sie krysztaly, które oczyszcza sie przez rozpuszczenie w benzolu.Nowy kwas zawiera prócz arsenu jeszcze brom. Tworzy on krysztaly zól¬ tawo—brunatne, topniejace przy 255-258°.Krysztaly te nie rozpuszczaja sie w wo¬ dzie, sa prawieni erozpuszczalne w eterze naftowym, rozpuszczaja sie natomiast w acetonie i benzolu.Jezeli rozpuszcza sie kwas ten, jak w przykladzie 1, w lugu potasowym przy 0°, i wprowadza kwas weglowy, otrzymuje sie opisana y przykladzie 1 kwasna sól potasowa.Jezeli zastapi sie lug potasowy lugiem sodowym, powstaje odpowiednia kwasna sól sodowa.Produkty maja zastosowanie w terapji. PLThe main German patent 257641 and additional patents 268829, 271159 and 273219 describe methods for the preparation of arsenic-containing fatty acids and their derivatives, consisting in the fact that acethylene acids or their derivatives are subjected to the action of arsenic tri-halogen derivatives or mixtures of , producing these derivatives, relatively reacting like them. It has been found that, in contrast to the amorphous products obtained in this way, it is possible to obtain nicely crystallized bodies if the phenylpropyl acid is subjected to the reactions described in given patents. The arsenic-containing derivative of phenylpropiolic acid obtained in this way is characterized, apart from its crystallization properties, by easy susceptibility to separation of the halogen under the action of weak alkalis, while also crystalline salts are obtained. Example 1. 20 parts by weight of phenylpropiolic acid are heated in 50 parts by weight of arsenic trichloride in 24 hours to 100 °. On standing or adding ether, lamellar crystals separate from the reaction fluid, which, after filtering off, washing with ether and recrystallization, are completely colorless and contain approximately 14.5% chlorine and approximately 16% arsenic. They are insoluble in water, but dissolve in hot acetone, chloroform and benzol, more difficult in ether. If 15 parts of this acid are dissolved in 120 parts one and a half times the normal potassium liquor at 0 ° and it enters the given in the case of the permeated liquid, carbonic acid separates as a crystalline slurry, a crystalline potassium acid salt with water content. After recrystallization from 10 times the amount of hot water and removal of the water of crystallization, it contains about 17% of arsenic, dissolves easily in cold alkali or alkaline carbonates, and when heated in excess of alkali in a water bath, releases arsenous acid EXAMPLE 2 50 parts by weight of phenylpropiolic acid are heated in 200 parts of arsenic tribromide to 100 ° for 20 hours. The reaction mass is dissolved in a small amount of ether and a small amount of petroleum ether is added. Crystals are formed which are purified by dissolving in benzol. The new acid contains, apart from arsenic, also bromine. It forms yellowish-brown crystals, melting at 255-258 °. These crystals do not dissolve in water, they are almost erodible in petroleum ether, but they dissolve in acetone and benzene. If this acid is dissolved, as in the example 1, in potassium liquor at 0 °, and introducing carbonic acid, one obtains the 1 acid potassium salt described in the example. If the potassium liquor is replaced with sodium liquor, the corresponding acidic sodium salt is obtained. PL
Claims (1)
Publications (1)
| Publication Number | Publication Date |
|---|---|
| PL366B1 true PL366B1 (en) | 1924-07-30 |
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