HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 59309864, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Diisobutylaluminumhydride | HCID 21225700 | — |
| Reactant | HCID 25056523 | HCID 25056523 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 59309864 | HCID 59309864 | 78.5% |
Reaction Steps
To a solution of 3-[2-chloro-5-(2,3,4,5-tetrahydro-1H-1-benzoazepin-1-ylsulfonyl)-phenyl]-5-ethoxycarbonyl-7-methyl-1,3-dihydro-2H-imidazo[4,5-b]pyridin-2-one (87 mg) in tetrahydrofuran (1.6 mL) was added diisobutylaluminium hydride (0.99 mol/L toluene solution, 0.65 mL) under ice-cooling, and the mixture was stirred at room temperature overnight. To the reaction mixture was added 1 mol/L hydrochloric acid, and the resulting mixture was extracted with ethyl acetate. The extract was washed with brine, and dried over anhydrous magnesium sulfate. The solvent was removed under reduced pressure, and the residue was purified by column chromatography on silica gel (eluent: n-hexane−ethyl acetate) to give the title compound (63 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08217069B2 |
| Source dataset | uspto-grants-2012_07 |
| ORD ID | ord-7b6dd03469654caaa63027078d2534b9 |
| Source note | uspto-grants-2012_07 |