HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 5.6-Dichloro-3-(2-(S)-azetidinylmethoxy)pyridine hydrochloride
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 5,6-Dichloro-3-(2-(S)-azetidinylmethoxy)pyridine | HCID 10263376 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | 5.6-Dichloro-3-(2-(S)-azetidinylmethoxy)pyridine hydrochloride | HCID 21309706 | 162.2% |
Reaction Steps
The compound from step 109c (338 mg, 1.45 mmol) was slurried in ether (15 mL), and ether saturated with HCl gas was added. Solvent was removed and the remaining white solid was recrystallized from methanol/Et2O to give 317 mg of short white needles, 81% yield. m.p.=181-182° C. MS (CI) m/e 233 (M+H)+. 1H NMR (D2O, 300 MHz) δ: 8.13 (d, J=2.9 Hz, 1H), 7.79 (d, J=2.9 Hz, 1H), 4.99-4.91 (m, 1H), 4.44 (d, J=4.4 Hz, 2H), 4.21-4.03 (m, 2H), 2.74-2.65 (m, 2H). Anal. calc. for C9H11Cl3N2O: C, 40.10; H, 4.11; N, 10.39; Found: C, 39.89; H, 4.08; N, 10.25.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05948793 |
| Source dataset | uspto-grants-1999_09 |
| ORD ID | ord-51da3c924fd8487abc51a4d5c4ea9c28 |
| Source note | uspto-grants-1999_09 |