HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → HCID 11554980, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | HCID 68546370 | HCID 68546370 | — |
| Catalyst | Palladium hydroxide | HCID 9942167 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 11554980 | HCID 11554980 | 18% |
Reaction Steps
A slurry of the the product of step (e) (105 mg) and palladium hydroxide (100 mg) in a solution of 1:1 acetic acid:tetrahydrofuran (10 mL) was stirred under an atmosphere of hydrogen for 24 h. The catalyst was filtered off, the filtrate evaporated and the residue purified by reverse phase HPLC to afford the title compound (16 mg) in the form of a white solid as a trifluoroacetate salt. m/z: [M+H+] calcd for C31H28N2O4, 493.2. found 493.5. 1H NMR (300 MHz, DMSO-d6): 10.40 (d, 1H, J=20 Hz), 8.60 (br s, 1H), 8.01 (d, 1H, J=8.8 Hz), 7.49 (d, 2H, J=8.2 Hz), 7.14-7.34 (m, 7H), 7.03 (d, 1H, J=7.4 Hz), 6.93 (d, 2H, J=7.4 Hz), 6.86-6.82 (m, 2H), 6.46 (d, 1H, J=9.9 Hz), 6.07 (s, 1H), 5.18 (m, 1H), 3.19-2.82 (m, 6H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07317023B2 |
| Source dataset | uspto-grants-2008_01 |
| ORD ID | ord-0610ece17a9e48b8b94918cf6b4e4b0a |
| Source note | uspto-grants-2008_01 |