HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 67993162, compound → HCID 67993074, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 67993162 | HCID 67993162 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Trifluoroacetic acid | HCID 6422 | — |
| Product | HCID 67993074 | HCID 67993074 | 70.2% |
Reaction Steps
To a solution of 9a (0.7 g, 2.3 mmol) in CH2Cl2 (15 mL), TFA (2 mL) was added. The reaction mixture was stirred at room temperature for 4 h. The solvent was removed under reduced pressure and the residue was neutralized with aqueous NaOH solution and extracted with CH2Cl2 (2×15 mL). The organic layer was washed with brine, dried and concentrated to give the crude product. The crude product was purified with column chromatography to afforded 10a (0.33 g, 70%). 1H NMR (CDCl3): δ 1.62-1.87 (m, 6H), 2.63 (s, 3H), 2.77 (m, 2H), 3.16-3.22 (m, 2H), 3.33 (m, 1H), 7.27 (d, J=8.4 Hz, 1H), 8.12 (dd, J=8.1, 2.4 Hz, 1H), 9.04 (d, J=2.4 Hz, 1H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08658131B2 |
| Source dataset | uspto-grants-2014_02 |
| ORD ID | ord-7b37dcdf4d0742f3b6fa66dbe18d4092 |
| Source note | uspto-grants-2014_02 |