HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Hydroxide → HCID 178526709, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Hydroxide | HCID 14797 | — |
| Reactant | 6-chloro-3-nitro-N-(tetrahydro-2H-pyran-4-yl)pyridin-2-amine | HCID 43610512 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 178526709 | HCID 178526709 | 98.4% |
Reaction Steps
6-Chloro-3-nitro-N-(tetrahydro-2H-pyran-4-yl)pyridin-2-amine (0.186 g, 0.722 mmol), 1 M aqueous potassium hydroxide solution (8.0 mL, 16.0 mmol) and dioxane (20 mL) were heated to 100° C. for 4 h. After cooling, the pH was adjusted to ˜7 and the mixture was extracted with EtOAc. The EtOAc extract was concentrated under reduced pressure to give the title compound (0.170 g). LCMS m/z=240.3 [M+H]+; 1H NMR (400 MHz, methanol-d4) δ ppm 1.65-1.80 (m, 2H), 2.05-2.15 (m, 2H), 3.60-3.70 (m, 2H), 4.00-4.10 (m, 2H), 4.20-4.30 (m, 1H), 5.92 (d, J=9.8 Hz, 1H), 8.32 (d, J=9.8 Hz, 1H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08507473B2 |
| Source dataset | uspto-grants-2013_08 |
| ORD ID | ord-3dd7edf10660472a9782d47c9fe4a6ed |
| Source note | uspto-grants-2013_08 |