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22nd September 2016 @ 17:43

The synthesis of 2-1 seemed to go well, but the purification did not go well, we we're making another attempt using the hydrazinylpyrazine sythesized here.

scheme

2-chloro-6-hydrazinyl pyrazine (0.36g, 2.55 mmol, 1 equiv) was added to a round-bottom flask with triethyl orthoformate (0.85 mL, 5.11 mmol, 2 equiv) and p-toluenesulfonic acid (97mg, 0.5 mmol, 0.2 equiv) in 7.5ml of toluene. This was dissolved and then heated to reflux for 24

TLC after 24 hours showed a significant amount of starting material left in the reaction mixture, so it was put in a microwave reactor for 30 minutes at 150 degrees in an effort to speed things along. This did not change the reaction mixture appreciably. NMR was attempted, but someone else's NMR tube broke in the probe, so the machine is down for the forseeable future.