HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 24769049, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Diethyl Ether | HCID 3283 | — |
| Reactant | HCID 86618075 | HCID 86618075 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 24769049 | HCID 24769049 | 28.5% |
Reaction Steps
To a solution of 23 (20 mg, 0.03 mmol) in dichloromethane (1 mL) under nitrogen was added dropwise a solution of 1N HCl in diethyl ether (2.0 mL, 2.0 mmol). The reaction mixture was stirred for 1 h at rt, concentrated in vacuo, and purified directly by HPLC (C-18 column, 10-70% gradient elution, MeCN:H2O with 0.1% TFA) to give 5 mg (25%) of the title compound. 1H NMR (400 MHz, DMSO-d6): δ 7.53 (s, 1H), 7.42 (dd, 1H), 7.15 (dd, 1H), 6.87 (dd, 1H), 5.88 (s, 2H), 4.79-4.72 (m, 1H), 4.53 (d, 2H), 4.48-4.46 (m, 4H), 4.15-4.07 (m, 2H), 3.88 (dd, 1H), 3.85 (s, 3H), 3.76 (dd, 1H), and 2.46 (s, 3H). MS 586 (M+1)+
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07776855B2 |
| Source dataset | uspto-grants-2010_08 |
| ORD ID | ord-b384a151d1114669a730bf2bf41a117a |
| Source note | uspto-grants-2010_08 |