please help me with the German procedure and translate it into English

Hi Jimmyapex

I am no chemist, but maybe this helps. The text translates to:

3.5g 5-nitro-2-aminopyridin were dissolved under heating (to 30°-40°C) in 56ml 48%HBr, and the mixture was then mixed with 16ml Br₂. This was then cooled to -5°C, 22g of NaNO₂ dissolved in 30ml H₂O was added such that the temperature stayed below 5°C. Then the mixture was stirred (until full completion of the reaction) for approximately 90 minutes (DC-control??) at 10° - 15°C, and then heated to around 40°C. After completion of the decomposition reaction (15 min) it was mixed into 200ml H₂O and the precipitate was sucked away. The produced 3.5g (67%) Raw Product were cleaned by recrystallisation out of CH₂OH, Melting point 139-140°C.

Good luck!

RKM

Honored sir, it is good try, but not entirely correct. German is tricky langage and its constructs are somehow different in upside down fashion.

I must apologize since I know but little German, but I think text should go:

3.5g 5-nitro-2-aminopyridin are to be dissolved under warming in 56ml 48% HBr heated to 30°-40°C and the solution is then fixed with 16ml Br₂. This was then cooled to -5°C and 22g of NaNO_2, dissolved in 30ml H₂O is added, taking care that the temperature stay below 5°C.

---------------------------------------------------------------------------------What follows may or may be not entirely correct as there are severall words I am not sure about........

In any case this is obviously dangerous chemical reaction, as witness cooling requirement, so whoever is working should have VERY PRECISE instruction!

Therefore droping out single word or imprecise translation can bring disaster!

Sometimes just difference in order of operations could bring disaster, like one acid (sorry, after 45 years I am not sure wether it was HydroCloric or Sulphuric acid) that ought be diluted by adding it drop by drop into wather and absolutely not opposite!

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Afterwards it ought to be stirred (carefuly?) about 90 min (DC-control??) untill total conversion is achieved with temperature of 10° - 15°C, and heated carefuly (or gradualy) on to around 40°C,

After fading away of the decomposition reaction and it is done and finished, it should be mixed with 200ml H2O and sediment has to be sucked away.

The produced 3.5g (67%) Raw Product has to be cleaned by recrystallisation using CH₂OH, on temperature of 139-140°C.

But still, I know little German, so I could be wrong, and ABSOLUTELY CORRECT translation is called for here, I would say!

One thing is sure, BABELFISH translated it still more badly and only less than half way, perhaps because I was unable to write correct Umlauts, special characters of Germam alfabet with two dots above letter.....