CH139411A - Process for the preparation of a crystallized arsenobenzene. - Google Patents
Process for the preparation of a crystallized arsenobenzene.Info
- Publication number
- CH139411A CH139411A CH139411DA CH139411A CH 139411 A CH139411 A CH 139411A CH 139411D A CH139411D A CH 139411DA CH 139411 A CH139411 A CH 139411A
- Authority
- CH
- Switzerland
- Prior art keywords
- arsenobenzene
- acid
- crystallized
- preparation
- salts
- Prior art date
Links
- 238000000034 method Methods 0.000 title claims description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 239000002253 acid Substances 0.000 claims description 5
- 150000003839 salts Chemical class 0.000 claims description 5
- 150000007659 semicarbazones Chemical class 0.000 claims description 5
- 239000011780 sodium chloride Substances 0.000 claims description 5
- LSNNMFCWUKXFEE-UHFFFAOYSA-M bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 claims description 3
- GQZXNSPRSGFJLY-UHFFFAOYSA-N Hypophosphorous acid Chemical compound OP=O GQZXNSPRSGFJLY-UHFFFAOYSA-N 0.000 claims description 2
- 230000001225 therapeutic Effects 0.000 claims description 2
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 claims 1
- 239000003638 reducing agent Substances 0.000 claims 1
- 229960000583 Acetic Acid Drugs 0.000 description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-N acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 2
- 239000012362 glacial acetic acid Substances 0.000 description 2
- ZGKNDXOLMOFEJH-UHFFFAOYSA-M Sodium hypophosphite Chemical compound [Na+].[O-]P=O ZGKNDXOLMOFEJH-UHFFFAOYSA-M 0.000 description 1
- 230000002378 acidificating Effects 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000004435 hydrogen atoms Chemical class [H]* 0.000 description 1
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910001379 sodium hypophosphite Inorganic materials 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Description
Verfahren zur Darstellung eines kristallisierten Arsenobenzols. In dem Hauptpatent ist ein Verfahren zur Darstellung eines kristallisierten Arseno- benzols aus dem Semicarbazon der 1-Benzal- dehyd-3-oxy-4-arsinsäure beschrieben.
Gegenstand dieser Erfindung ist ein Ver fahren zur Darstellung eines kristallisierten Arsenobenzols aus dem Semicarbazon des 1-Acetophenon - 3 - oxy-4-arsi noxyds, welches dadurch gekennzeichnet ist, dass man das Semicarbazon mit unterphosphoriger Säure und schwefliger Säure oder den Salzen dieser beiden Säuren sauer reduziert, wobei es zweck mässig sein kann, JodwasserstofEsäure- oder deren Salze in kleinen ATengen zuzusetzen.
Das erhaltene Arsenobenzol entspricht der Formel:
EMI0001.0017
und kristallisiert in spitzen Nädelchen, welche sich gegen 230 zersetzen und in verdünnter Natronlauge leicht löslich sind.
Es soll zu therapeutischen Zwecken Ver wendung finden.
<I>Beispiel</I> 0,3 gr Semicarbazon des 1-Acetophenon- 3-oxy-4-arsin-oxyds werden in einer Eisessig Natriumhypophosphitlösung 1 : 10 suspendiert und versetzt mit 0,5-1 cm3 wässeriger schwef liger Säure (1 em3 = 0,68-0,70 cm!' n NaOH). Die möglichst vollständig angefüllte Druck flasche wird bei gewöhnlicher Temperatur mehrere Stunden geschüttelt oder kurze Zeit bis auf 70 erwärmt. Die anfangs weisse Suspension wandelt sich in ein prachtvoll in spitzen Nädelchen kristallisierendes Arseno- benzol um.
Nach dem Absaugen wird mit wenig Eisessig und darauf mit Wasser nach gewaschen. Das Arsenobenzol löst sich leicht in verdünnter Natronlauge auf und zersetzt sich gegen 230 .
Process for the preparation of a crystallized arsenobenzene. The main patent describes a process for preparing a crystallized arsenobenzene from the semicarbazone of 1-benzaldehyde-3-oxy-4-arsic acid.
This invention relates to a process for the preparation of a crystallized arsenobenzene from the semicarbazone of 1-acetophenone - 3 - oxy-4-arsi noxyds, which is characterized in that the semicarbazone with hypophosphorous acid and sulfurous acid or the salts of these two acids acidic reduced, whereby it may be useful to add hydrogen iodine acid or salts thereof in small amounts.
The arsenobenzene obtained corresponds to the formula:
EMI0001.0017
and crystallizes in sharp needles, which decompose towards 230 and are easily soluble in dilute sodium hydroxide solution.
It should be used for therapeutic purposes.
<I> Example </I> 0.3 g semicarbazone of 1-acetophenone-3-oxy-4-arsine oxide are suspended in a glacial acetic acid sodium hypophosphite solution 1:10 and mixed with 0.5-1 cm3 aqueous sulfurous acid ( 1 em3 = 0.68-0.70 cm! 'N NaOH). The pressure bottle, filled as completely as possible, is shaken at normal temperature for several hours or heated up to 70 for a short time. The initially white suspension is transformed into arsenobenzene, which crystallizes splendidly in sharp needles.
After suctioning off, it is washed with a little glacial acetic acid and then with water. The arsenobenzene dissolves easily in dilute sodium hydroxide solution and decomposes around 230.
Claims (1)
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE139411X | 1926-09-06 | ||
CH130795T | 1927-09-02 |
Publications (1)
Publication Number | Publication Date |
---|---|
CH139411A true CH139411A (en) | 1930-04-15 |
Family
ID=25711505
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CH139411D CH139411A (en) | 1926-09-06 | 1927-09-02 | Process for the preparation of a crystallized arsenobenzene. |
Country Status (1)
Country | Link |
---|---|
CH (1) | CH139411A (en) |
-
1927
- 1927-09-02 CH CH139411D patent/CH139411A/en unknown
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