HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 86682912, compound → HCID 86682911, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 86682912 | HCID 86682912 | — |
| Solvent | Hydrochloric Acid | HCID 313 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 86682911 | HCID 86682911 | 25.9% |
Reaction Steps
To a solution of {2-(4-iodo-phenyl)-6-(tetrahydro-pyran-2-yloxy)-3-[4-(tetrahydro-pyran-2-yloxy)-phenyl]-4-trifluoromethyl-chroman-4-yloxy}-trimethyl-silane (15 g, 73 mmol) in MeOH (400 mL), concentrated HCl (100 mL) was added. The reaction mixture was stirred at room temperature for 4 h, concentrated, and re-dissolved in DCM (150 mL). The solution was washed (3×100 mL brine), dried (Na2SO4), filtered, and concentrated. The residue was purified by silica gel column chromatography (PE/EA=10/1) to afford the desired product (10 g). 1H NMR (DMSO-d6): δ 9.17 (s, 1H), 9.08 (s, 1H), 7.55 (d, 2H), 7.10 (d, 2H), 7.06-6.99 (m, 3H), 6.76-6.65 (m, 2H), 6.55-6.48 (m, 3H), 5.77 (d, 1H), 3.55 (d, 1H); LCMS: 527 (M−H)−.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08703810B2 |
| Source dataset | uspto-grants-2014_04 |
| ORD ID | ord-da8a1210017a43faad2df54210080a17 |
| Source note | uspto-grants-2014_04 |