HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 3-Pyridazinamine, 6-methyl-4-(1-methylethyl)-
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | N-[4-(1-methylethyl)-6-methyl-pyridazin-3-yl]-2,2-dimethyl-propionamide | HCID 68858996 | — |
| Product | 3-Pyridazinamine, 6-methyl-4-(1-methylethyl)- | HCID 45116643 | 67% |
Reaction Steps
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.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07557103B2 |
| Source dataset | uspto-grants-2009_07 |
| ORD ID | ord-35f6e308f3c14c7eb58dd5fe0867d5aa |
| Source note | uspto-grants-2009_07 |