反应详情

A solution of 3,6-diethyl-N-(1-ethylpropyl)pyrazin-2-amine, NIS (5.37 g, 23.9 mmol) and anhydrous DMF (100 mL) under N2 was heated at 50° C. for 4 h. The solution was partitioned between ethyl acetate and H2O and separated. The aqueous phase was extracted with ethyl acetate and the combined organics were washed with H2O, brine and dried (MgSO4). The mixture was filtered and concentrated to give a brown oil which was purified by flash chromatography (20% ethyl acetate in heptane) to give 5.57 g (74%) of 3,6-diethyl-N-(1-ethylpropyl)-5-iodopyrazin-2-amine as a light brown oil. 1H NMR (400 MHz, CDCl3) δ 4.02 (m, 2 H), 2.76 (q, 2 H), 2.57 (q, 2 H), 1.60-1.70 (m, 2 H), 1.45-1.55 (m, 2 H) 1.20-1.30 (m, 6 H), 0.92 (q, 6 H).

1. customThe solution was partitioned between ethyl acetate and H2O
2. customseparated
3. extractionThe aqueous phase was extracted with ethyl acetate
4. washthe combined organics were washed with H2O, brine
5. dry with materialdried (MgSO4)
6. filtrationThe mixture was filtered
7. concentrationconcentrated
8. customto give a brown oil which
9. customwas purified by flash chromatography (20% ethyl acetate in heptane)