HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloride methanol → HCID 71523146, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloride methanol | HCID 21893726 | — |
| Reactant | HCID 89524677 | HCID 89524677 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 71523146 | HCID 71523146 | — |
Reaction Steps
To a solution of Example 140C (390 mg, 0.866 mmol) in MeOH (2 mL) was added HCl/MeOH (2 M, 2 mL, 4 mmol) at room temperature. The reaction mixture was stirred at ambient temperature overnight. The solvent was removed in vacuo. The resulting residue was partitioned between EtOAc (20 mL) and saturated NaHCO3 (20 mL). The organic layer was separated, dried over Na2SO4, filtered, and concentrated. Crude product was purified by Prep-HPLC (Column: Waters X-bridge ODS C18 21.2×250 mm, water (0.05% TFA): acetonitrile 45-85%) to give Example 140D. LCMS: 450[M+1]. 1H NMR (400 MHz, DMSO-d6): δ 12.81 (s, 1H), 7.76 (s, 1H), 7.63 (d, J=7.6 Hz, 1H), 7.37-7.46 (m, 3H), 7.20 (d, J=16.0 Hz, 1H), 2.61 (s, 3H), 2.37 (s, 3H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08772500B2 |
| Source dataset | uspto-grants-2014_07 |
| ORD ID | ord-c3b1788e62024dbdae5a45f43c0d98be |
| Source note | uspto-grants-2014_07 |