HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 16659814, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | HCID 16659815 | HCID 16659815 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 16659814 | HCID 16659814 | 201.2% |
Reaction Steps
A solution of (E)-3-(6-amino-pyridin-3-yl)-N-(3-chloro-4-fluoro-benzo[b]thiophen-2-ylmethyl)-N-methylacrylamide (257 mg, 0.68 mmol) in CH2Cl2 (10 mL) was treated with anhydrous HCl (0.68 mL of a 1.0 M solution in Et2O, 0.68 mmol). The mixture was stirred overnight at room temperature and then diluted with Et2O. The resulting solid was collected by filtration and then dried under vacuum at 50° C. for 2 d to give the title compound (282 mg, 98%) as an off-white solid and as a mixture of amide rotamers: 1H NMR (300 MHz, DMSO-d6) δ 8.43-8.33 (m, 4H), 7.87-7.82 (m, 1H), 7.55-7.20 (m, 4H), 7.04-7.00 (m, 1H), 5.15-4.88 (m, 2H), 3.54 (br s, 1H), 3.22-2.97 (m, 3H); MS (ESI) m/e 376 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08450307B2 |
| Source dataset | uspto-grants-2013_05 |
| ORD ID | ord-220b80d8f1d9483682774d7d4b41fe53 |
| Source note | uspto-grants-2013_05 |