HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dichloromethane → HCID 58269303, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | HCID 58269240 | HCID 58269240 | — |
| Reactant | HCID 178418361 | HCID 178418361 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 58269303 | HCID 58269303 | 38% |
Reaction Steps
To a solution of example 21 (0.080 g, 0.173 mmoles) in methanol (10 ml), palladium on carbon (10% 16 mg) was added and the solution was hydrogenated at RT under 5 kg/cm2 pressure of hydrogen for 24 h. The solution was filtered through celite and concentrated. The crude product was purified by column chromatography with methanol: dichloromethane to afford the title compound as light yellow solid (0.025 g, 38% yield). MP: 254-257° C. 1H-NMR (δ ppm, DMSO-D6, 400 MHz): δ 8.46(s, 1H), 8.03(s, 1H), 8.01(d, J=1.6 Hz, 1H), 7.83(dt, J=7.3,1.7 Hz, 1H), 7.65 (d, J=8.2 Hz, 1H), 7.50 (m, 4H), 7.37(dd, J=8.1,1.7 Hz, 1H),7.22(s, 2H), 5.67(q, J=7.3 Hz, 1H),1.89(d, J=7.2 Hz, 3H).). Mass: 384.19(M+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08642607B2 |
| Source dataset | uspto-grants-2014_02 |
| ORD ID | ord-f1ce31bd5cee44178fa2fb53b8d871d5 |
| Source note | uspto-grants-2014_02 |