HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 24768826, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Diethyl Ether | HCID 3283 | — |
| Reactant | HCID 24768888 | HCID 24768888 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 24768826 | HCID 24768826 | 36.2% |
Reaction Steps
To a solution of 9 (50 mg, 0.08 mmol) in CH2Cl2 (2 mL) under nitrogen was added 1N HCl in Et2O (2.0 mL, 2.0 mmol). The reaction mixture was stirred at rt for 2 h, concentrated in vacuo, and purified directly by HPLC (C-18 column, 30-80% gradient elution, MeCN:H2O with 0.1% TFA). Fractions containing product were lyophilized to give 15 mg (36%) of the title compound as the trifluoroacetate salt. 1H NMR (400 MHz, DMSO-d6): δ 9.07 (br s, 1H), 7.54 (s, 1H), 7.43 (dd, 1H), 7.16 (dd, 1H), 6.87 (dd, 1H), 5.96-5.92 (m, 2H), 4.80-4.74 (m, 1H), 4.48-4.46 (m, 4H), 4.15-4.09 (m, 4H), 3.91 (dd, 1H), 3.85 (s, 3H), 3.76 (dd, 1H), 2.62 (s, 3H), 2.47 (s, 3H). MS 519 (M+1)+
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07776855B2 |
| Source dataset | uspto-grants-2010_08 |
| ORD ID | ord-b568425f5746464faa92058922368516 |
| Source note | uspto-grants-2010_08 |