HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 68769938, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Lithium Hydroxide | HCID 3939 | — |
| Reactant | HCID 131728424 | HCID 131728424 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Solvent | Oxolane--water (1/1) | HCID 21881883 | — |
| Product | HCID 68769938 | HCID 68769938 | 64.2% |
Reaction Steps
To a solution of Example 17B (55 mg, 0.13 mmol) in a mixture of tetrahydrofuran/H2O (1.0 mL/0.5 mL), LiOH (19 mg, 0.80 mmol) was added at room temperature. The reaction mixture was stirred overnight. It was acidified with 2N HCl in ether until pH=3 and purified by high pressure liquid chromotography (eluting with 0-70% acetonitrile/water and 0.1% trifluoroacetic acid) to provide the title compound (32 mg, 63%). 1H NMR (400 MHz, methanol-d4) δ ppm 7.78 (s, 1H), 7.55-7.52 (m, 1H), 7.42-7.38 (m, 1H), 6.21 (s, 1H), 4.0-3.90 (m, 1H) 3.85-3.70 (m, 2H), 3.65-3.50 (m, 1H), 3.20-2.8 (m, 3H), 2.75-2.55 (m, 3H), 2.50-2.40 (m, 3H), 2.35-2.20 (m, 2H), 2.05-1.85 (m, 2H). MS (APCI) m/z 383 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07834012B2 |
| Source dataset | uspto-grants-2010_11 |
| ORD ID | ord-af209da677fa43ca8257ea4270eafee6 |
| Source note | uspto-grants-2010_11 |