CH158826A - Process for the preparation of 9-methyl-2-oxycarbazole-3-carboxylic acid. - Google Patents
Process for the preparation of 9-methyl-2-oxycarbazole-3-carboxylic acid.Info
- Publication number
- CH158826A CH158826A CH158826DA CH158826A CH 158826 A CH158826 A CH 158826A CH 158826D A CH158826D A CH 158826DA CH 158826 A CH158826 A CH 158826A
- Authority
- CH
- Switzerland
- Prior art keywords
- methyl
- oxycarbazole
- carboxylic acid
- preparation
- acid
- Prior art date
Links
Description
Verfahren zur Darstellung von 9-Nethyl-2-oayearbazol-3-earbonsäure. Es wurde gefunden, dass man 9-Methyl- 2-oxycarbazol-3-carbonsäure dadurch erhalten kann, dass man 9-Methyl-2-oxycarbazol in Gegenwart eines Alkalis bei erhöhter Tem peratur mit Kohlensäure unter Druck behan delt und die freie Säure aus ihrem Alkali salz abscheidet, zum Beispiel mit Hilfe einer Mineralsäure. Die 9-Methyl-2-oxycarbazol-3- carbonsäure kristallisiert aus Toluol oder Alkohol in farblosen Nadeln vom Schmelz punkt 239 bis 240' C.
Sie ist ein wertvolles Zwischenprodukt zur Herstellung von Farb stoffen. <I>Beispiel:</I> 19,7 Gewichtsteile 9-Methyl-2-oxycarba- zol (I"Tadeln aus verdünntem Alkohol vom Achmelzpunkt 167 bis<B>168</B> ) werden mit 13,6 Gewichtsteilen 30%iger Natronlauge ver rührt und durch Erhitzen entwässert. Das so entstandene Natronsalz wird in einen Autoklaven eingefüllt und mit Glasperlen vermischt.
Unter einem Kohlensäuredruck von etwa 15 Atmosphären wird der Autoklav während 6 Stunden auf etwa 220' Innen temperatur erhitzt. Nach Erkalten lässt man den Kohlensäuredruck ab, kocht den Auto klavenrückstand mit Wasser aus und leitet Kohlensäure ein, um eventuell vorhandene geringe Mengen von unverändertem Oxykör- per auszufällen. Aus der filtrierten Lösung fällt durch Zusatz von Mineralsäuren diP neue Oxycarbonsäure aus.
Sie kristallisiert aus Toluol oder Alkohol in farblosen Nadeln vom Schmelzpunkt 239 bis 240'. Die alko holische Lösung färbt sich beim Zusatz von Eisenchlorid kräftig blau an.
Process for the preparation of 9-Nethyl-2-oayearbazol-3-carboxylic acid. It has been found that 9-methyl-2-oxycarbazole-3-carboxylic acid can be obtained by treating 9-methyl-2-oxycarbazole in the presence of an alkali at elevated temperature with carbonic acid under pressure and treating the free acid from it Separates alkali salt, for example with the help of a mineral acid. The 9-methyl-2-oxycarbazole-3-carboxylic acid crystallizes from toluene or alcohol in colorless needles with a melting point of 239 to 240 ° C.
It is a valuable intermediate product in the manufacture of dyes. <I> Example: </I> 19.7 parts by weight of 9-methyl-2-oxycarba- zole (I "blame from dilute alcohol from a melting point of 167 to <B> 168 </B>) with 13.6 parts by weight of 30% Sodium hydroxide solution is stirred and dehydrated by heating.The resulting sodium salt is poured into an autoclave and mixed with glass beads.
Under a carbonic acid pressure of about 15 atmospheres, the autoclave is heated to about 220 'internal temperature for 6 hours. After cooling down, the carbonic acid pressure is released, the autoclave residue is boiled out with water and carbonic acid is introduced in order to precipitate any small amounts of unchanged oxy body that may be present. New oxycarboxylic acid precipitates from the filtered solution by adding mineral acids diP.
It crystallizes from toluene or alcohol in colorless needles with a melting point of 239 to 240 '. The alcoholic solution turns a strong blue when iron chloride is added.
Claims (1)
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE158826X | 1931-01-12 | ||
| CH158826T | 1932-01-05 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CH158826A true CH158826A (en) | 1932-12-15 |
Family
ID=25717148
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CH158826D CH158826A (en) | 1931-01-12 | 1932-01-05 | Process for the preparation of 9-methyl-2-oxycarbazole-3-carboxylic acid. |
Country Status (1)
| Country | Link |
|---|---|
| CH (1) | CH158826A (en) |
-
1932
- 1932-01-05 CH CH158826D patent/CH158826A/en unknown
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