HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 49780164, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | HCID 49780163 | HCID 49780163 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 49780164 | HCID 49780164 | 89% |
Reaction Steps
Intermediate 41 (2.02 g, 5.0 mmol) was treated with 1M HCl in methanol (35 mL) and refluxed for 3 hours. The solvent was evaporated and the residue diluted with 1N NaOH. The resulting precipitate was removed by filtration and further dried under high vacuum to give intermediate 42 (1.35 g, 89%) as a white solid: Mp 169-173° C. 1H NMR (500 MHz, DMSO-d6) δ 8.49 (s, 1H), 7.46 (d, J=9.0 Hz, 2H), 7.21 (d, J=8.6 Hz, 2H), 6.15 (d, J=7.7 Hz, 1H), 3.55-3.45 (m, 1H), 2.89 (td, J=12.8, 3.5 Hz, 2H), 2.49-2.45 (m, 2H), 2.13 (s, 1H), 1.74 (dd, J=12.4, 2.4 Hz, 2H), 1.21 (dq, J=11.7, 3.7 Hz, 2H). HRMS calculated for C13H16F3N3O2−H+ 302.1117. found (ESI(−), [M−H]) 302.1114.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09296693B2 |
| Source dataset | uspto-grants-2016_03 |
| ORD ID | ord-995633b882af43ddaa081473af61d784 |
| Source note | uspto-grants-2016_03 |