HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 68772375, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Lithium Hydroxide | HCID 3939 | — |
| Reactant | Oxolane--water (1/1) | HCID 21881883 | — |
| Reactant | HCID 68768163 | HCID 68768163 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | HCID 68772375 | HCID 68772375 | 80.6% |
Reaction Steps
To a solution of Example 9B (18 mg, 0.037 mmol) in mixture of tetrahydrofuran/H2O (0.5 mL/0.25 mL), LiOH (9.4 mg, 0.22 mmol) was added at room temperature. The reaction mixture was stirred overnight. It was acidified with 2N HCl in ether until the pH=3 and purified by reverse-phase high pressure liquid chromotography (eluting with 0-70% acetonitrile/water and 0.1% trifluoroacetic acid) to provide the title compound (14 mg, 80%). 1H NMR (500 MHz, methanol-d4) δ ppm 8.65-8.76 (m, 2H), 8.25-8.33 (m, 1H), 7.81-7.91 (m, 1H), 7.48-7.65 (m, 3H), 7.30-7.44 (m, 3H), 7.01-7.10 (m, 1H), 4.48-4.59 (m, 2H), 4.00-4.12 (m, 1H), 3.74-3.87 (m, 1H), 2.60-3.02 (m, 4H). MS (ESI) m/z 469 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07834012B2 |
| Source dataset | uspto-grants-2010_11 |
| ORD ID | ord-fa6d358392d048e083ac82aced5ba09d |
| Source note | uspto-grants-2010_11 |