Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 66976385 | HCID 66976385 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 66975082 | HCID 66975082 | 114.8% |
Reaction Steps
To a solution of tert-butyl (6R,7R)-7-(4-chloro-3-fluorophenyl)-6-({[(3-chloropropyl)carbamoyl]amino}methyl)-1,4-oxazepane-4-carboxylate (531 mg) in DMF (22 mL) was added sodium hydride (48.8 mg, 60% in oil) under ice-cooling, and the mixture was stirred at 0° C. for 2 hr. To the reaction mixture was added distilled water, and the mixture was extracted with ethyl acetate. The extract was washed with distilled water and brine, and dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel chromatography (hexane/ethyl acetate) to give the title compound (563 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US08722662B2 |
|---|
| Source dataset | uspto-grants-2014_05 |
|---|
| ORD ID | ord-32a2735ffd704c19b72fcaddfc24cfb2 |
|---|
| Source note | uspto-grants-2014_05 |
|---|