反应详情

N-[4-(1-methylethyl)-6-methyl-pyridazin-3-yl]-2,2-dimethyl-propionamide (1.38 g, 5.87 mmol) is treated with HCl 0 (10 mL), and refluxed for 3 h. It is cooled to rt, poured into ice-H2O (30 mL); extracted with EtOAc (2×30 mL). The aqueous layer is treated with 5 M NaOH to adjust the pH to 8-9. It is then extracted with EtOAc (3×50 mL); dried with Na2SO4, filtered and concentrated gives the title compound (0.59 g, 3.91 mmol, 67%). %). 1H NMR (CDCl3): δ 1.28 (d, J=7.0 Hz, 6H), 2.51 (s, 3H), 2.72-2.83 (m, 1H), 5.95 (bs, 2H), 7.02 (s, 1H) ppm. ES-MS (m/z): calcd for C8H13N3 (M+H)+: 152.2. found: 152.1.

1. temperaturerefluxed for 3 h
2. extractionextracted with EtOAc (2×30 mL)
3. additionThe aqueous layer is treated with 5 M NaOH
4. extractionIt is then extracted with EtOAc (3×50 mL)
5. dry with materialdried with Na2SO4
6. filtrationfiltered
7. concentrationconcentrated