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30th September 2014 @ 01:13

See Repeat synthesis of 5-chloro-[1,2,4]triazolo[4,3-a]pyrazine (TM 37-14) for method.

scheme

hydrazinylpyrazine (from Preparation of 2-hydrazinylpyrazine (TM 62-1): 1.5 g, 13.6 mmol) was dissolved in toluene (15 mL), triethyl orthoformate (3.4 ml, 20.4 mmol, 1.5 eq) and TsOH (235 mg, 1.36 mmol, 10 mol %) added, and the reaction mixture refluxed (bath temp 110 oC) for 24 h. Solvents removed under reduced pressure, around half the the reaction mixture was lost by knocking over the flask, and the remainder was purified by FCC (EtOAc, hexanes) to give 345 mg (2.9 mmol, 22 %, see above) of pure TM 65 as a yellow powder.

 

 

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