HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 11978592, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Ethanol | HCID 702 | — |
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | HCID 67109309 | HCID 67109309 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 11978592 | HCID 11978592 | 51% |
Reaction Steps
A mixed solution of N-[4-fluoro-1-(methoxymethoxy)-2-(1,3-thiazol-2-yl)-1H-indol-7-yl]-N-methylthiophene-2-sulfonamide (165 mg), 6N hydrochloric acid (6 mL), tetrahydrofuran (2 mL) and ethanol (4 mL) was stirred at 80° C. for 7 hr. The reaction solution was diluted with ethyl acetate, washed with water, aqueous sodium hydrogencarbonate solution and saturated brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The obtained residue was subjected to silica gel column chromatography (ethyl acetate:hexane=1:9-3:7), and the obtained crystals were recrystallized from ethyl acetate-hexane to give the title compound (73 mg, yield 49%) as colorless needle crystals. melting point 197-198° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08957070B2 |
| Source dataset | uspto-grants-2015_02 |
| ORD ID | ord-75bb9c6d5ca241d5b746f14bd2f7c162 |
| Source note | uspto-grants-2015_02 |