HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → HCID 91446597, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | HCID 91523691 | HCID 91523691 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 91446597 | HCID 91446597 | 13% |
Reaction Steps
A mixture of Example 656A (20 mg, 0.04 mmol) in acetic acid (1 mL) and water (200 μL) was heated at 100° C. overnight, cooled to room temperature, diluted with ethyl acetate, washed with water and brine, dried (MgSO4), filtered and concentrated. The concentrate was purified by preparative HPLC (2.5 mg, 13% yield). MS (ESI) m/e 482 (M+H)+; 1H NMR (400 MHz, DMSO-d.6 □ 11.67 (br s, 1H), 9.83 (s, 1H), 7.95 (s, 1H), 7.77 (d, J=8.1 Hz, 1H), 7.69 (dd, J=9.7, 2.5 Hz, 1H), 7.56 (m, 1H), 7.24-7.43 (m, 5H), 6.96 (d, J=8.1 Hz, 1H), 6.82-6.87 (m, 2H), 6.39 (d, J=9.2 Hz, 1H), 3.90 (s, 3H), 3.60 (s, 3H), 3.54 (s, 2H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07456169B2 |
| Source dataset | uspto-grants-2008_11 |
| ORD ID | ord-fe126762862e4227862345bda9d7eed7 |
| Source note | uspto-grants-2008_11 |