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Offline Woodwardt84

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German translation
« on: February 16, 2014, 04:08:05 PM »
Hi

Someone speaking german that can help me to translate this?

Thanks!!!

2-Amino-dihydroresorcin (III): Erhitzt man 20g (II) rnit 50ccm konz. Salzsaure 10 Min. auf dem kochenden Wasserbad, so fällt allmählich ein orangefarbener Niederschlag aus. Man entfernt die Salzsaure i. Vak. bei 50-60". trocknet den Riickstand Uber NaOH und P2O5 und kristallisiert aus 70ccm Eisessig um; als Rilckstand verbleiben 4.5 g oraogegelbe sich iiber- kreuzende Prismen vom Zen.-P. 235-240°. Die Substanz ist leicht lbslich in Wasser, Alko- hol; sehr schwer in Ather, Chloroform; unlaslich in Eisessig. Beilsteinprobe positiv. Zur Analyse wurde mit Eisessig ausgekocht.

Gef. C 49.26 H 5.70 N 8.79

Aus dem Filtrat fallt das Hydrochlorid des Amins in fast farblosen Nadeln. die abgesaugt, mit Eisessig und dann mit Xther gewaschen werden. Ausb. 7.6g (40% d. Th.). Beim Arbeiten in kleinerem MaOstab betragt die Ausbeute 50-55 %.
Das Hydrochlorid ist sehr leicht lbslich in Wasser und Alkohol; schwer in kaltem Eisessig; unlaslich in dither. An feuchter Atmosphare tritt ziemlich rasch Rosafarbung ein. Auch die trockene Substanz ist nur begrenzt haltbar und IaDt sich nicht titrieren. Zur Analyse wird aus HCI-haltigem Eisessig umkristallisiert. Das Hydrochlorid sintert ab 180"und schmilzt unter Zers. und Rotfarbung bei 229-230".

Offline discodermolide

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Re: German translation
« Reply #1 on: February 16, 2014, 08:20:53 PM »
1-Amino-dihydroresorcine (III): Compound (II), 20g, is treated with 50 mL of conc. hydrochloric acid by heating on a boiling water bath for 10 minutes. An orange coloured precipitate formed. The hydrochloric acid is removed by heating at 50-60+ under vacuum. The residue is dried over NaOH and P2O5 and re-crystallised from glacial acetic acid. Obtained are a orange-yellow prisms with MPt. 235-2440°C. The compound is very soluble in water and alcohol, slightly soluble in ether, chloroform  and insoluble in glacial acetic acid. Beilstein test positive. To obtain an analytical sample it was treated with with refluxing glacial acetic acid.
Found C49.26 H 5.7 N 8,79.

The amine hydrochloride precipitates out as almost colourless needles from the filtrate. These are collected by filtration, washed with glacial acetic acid and ether to give 7.6g, 40% of the theoretical yield. In small scale experiments the yield was 50-55%.
The hydrochloride is very soluble in water and alcohol; difficult to dissolve in cold glacial acetic acid and insoluble in ether. In moist air a pink colouration rapidly forms. Furthermore the dry compound is only stable for short periods and cannot be titrated. To obtain an analytical sample it was recrystallised from glacial acetic acid containing HCl.  The hydrochloride begins to sinter (bubble) at 180° and melts with decomposition at formation of a red colour at 229-230°C.
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