HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 24768947, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Diethyl Ether | HCID 3283 | — |
| Reactant | HCID 68468814 | HCID 68468814 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 24768947 | HCID 24768947 | 70.5% |
Reaction Steps
To a solution of 17a (500 mg, 0.78 mmol) in dichloromethane (2.5 mL) under an atmosphere of nitrogen was added a solution of 1N HCl in diethyl ether (2.34 mL, 2.34 mmol) and the reaction mixture was stirred at rt for 3 h. The reaction mixture was concentrated in vacuo, purified directly by HPLC (C-18 column, 10-100% gradient elution, MeCN:H2O), and fractions containing product were lyophilized to give 290 mg (70%) of the title compound. 1H NMR (400 MHz, DMSO-d6): δ 7.53 (s, 1H), 7.42 (dd, 1H), 7.16 (dd, 1H), 6.87 (dd, 1H), 5.65 (dd, 1H), 5.58 (dd, 1H), 4.87-4.80 (m, 1H), 4.48-4.46 (m, 4H), 4.20 (dd, 1H), 4.09 (dd, 1H), 3.87 (dd, 1H), 3.84 (s, 3H), 3.78 (dd, 1H), and 2.49 (s, 3H). MS 528 (M+1)+
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07776855B2 |
| Source dataset | uspto-grants-2010_08 |
| ORD ID | ord-1d7d5d89ce5843c29da83b210c351179 |
| Source note | uspto-grants-2010_08 |