HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 54413507, compound → HCID 54544963, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 54413507 | HCID 54413507 | — |
| Solvent | Hydrochloric Acid | HCID 313 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 54544963 | HCID 54544963 | 13% |
Reaction Steps
A solution of 28 mg (0,016 mmol) of the acetamide from Example 208 in 5 mL of methanol and 0.24 mL of 2N aqueous hydrochloric acid was heated at reflux for 3 days. It was then cooled and concentrated. Purification by HPLC (ODS-3, 1:1 methanol:0.1% aqueous trifluoroacetic acid) gave 6.7 mg (13%) the title compound as its bis trifluoracetate salt: 1H NMR (400 MHz, CD3OD) δ8.31 (d, 1H, J=1.5 Hz), 7.96-7.90 (m, 3H), 7.75 (dd, 1H, J=1.9, 8.7 Hz), 7.65-7.57 (m, 2H), 7.11 (s, 4H), 6.89 (s, 2H), 4.12 (m, 1H), 3.89 (dd, 1H, J=5.0, 9.9 Hz), 3.85 (dd, 1H, J=5.3, 9.9 Hz), 3.23-3.11 (m, 4 HO, 2.90-2.86 (m, 2H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05451677 |
| Source dataset | uspto-grants-1995_09 |
| ORD ID | ord-7112c66182cf4d87bc5ed7474bbd579c |
| Source note | uspto-grants-1995_09 |