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27th July 2015 @ 02:49
Desired product was obtained. Recrystalization failed. Reaction was discarded. Reaction started at 14:49. Reached temp at 15:05. Procedure 5-Chloro-[1,2,4]triazolo[4,3-a]pyrazine (1 g, 6.49 mmol) and NBS (2 g, 11.2 mmol, 1.7 equiv.) were placed in chloroform (50 mL) and refluxed for 24 h. The reaction mixture was diluted with chloroform (50 mL), washed with saturated carbonate solution (20mL). The aqueous layer was then re-extracted with chloroform (3*40mL). The combined organic was then washed with brine (40ml) and the solvent was removed under reduced pressure to give a brown solid. NMR of the crude showed that purification was needed. The solid was then purified by recrystallization in methanol (10ml) but did not dissolve well in methanol. Pale yellow solid was obtained. Ended up with mess. Reaction was discarded. Data NMR data of the crude: [data]15655[/data]  HIRAC  [data]15431[/data] Strings ClC1=CN=CC2=NN=CN21 to  ClC1=CN=CC2=NN=C(Br)N21 InChI=1S/C5H3ClN4/c6-4-1-7-2-5-9-8-3-10(4)5/h1-3H to InChI=1S/C5H2BrClN4/c6-5-10-9-4-2-8-1-3(7)11(4)5/h1-2H
Attached Files
HIRAC TZ 4-1.pdf
TZ 4-1 crude.pdf
TZ 4-1 crude.rar