HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 69508390, compound → HCID 10429577, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 69508390 | HCID 69508390 | — |
| Solvent | Sodium Hydroxide | HCID 14798 | — |
| Solvent | Methanol--water (1/1) | HCID 22242641 | — |
| Product | HCID 10429577 | HCID 10429577 | 36.5% |
Reaction Steps
The ester from Example 10C (65 mg, 0.16 mmol) was dissolved in 4M NaOH (5 mL) in MeOH/H2O (5:3). After 2 hours no starting material was visible by TLC. When the reaction mixture was acidified to pH 1, the product precipitated out. The titled compound (22 mg, 36%) was obtained after reverse phase HPLC (0–70% acetonitrile in 0.1% aqueous TFA) as a white solid. MS (DEI) positive ion; m/z 376 (M)+: negative ion; m/z 751.1 (2M−H)−, 375.1 (M−H)−. 1H NMR (300 MHz, DMSO-d6) δ 7.6 (s, 2H), 7.7 (t, J=7.8 Hz, 2H), 8.0 (dd, J=8.1, 1.5 Hz, 4H), 8.3 (s, 2H), 14.0 (br s, 2H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07169797B2 |
| Source dataset | uspto-grants-2007_01 |
| ORD ID | ord-e7bb8ced963c4921bf28723bed887805 |
| Source note | uspto-grants-2007_01 |