HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 59722591, compound → HCID 59722729, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 59722591 | HCID 59722591 | — |
| Reactant | HCID 178418573 | HCID 178418573 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 59722729 | HCID 59722729 | 82.5% |
Reaction Steps
Methylmagnesium bromide (3.0 M in ether; 0.70 mL, 2.10 mmol) was added to a solution of tert-butyl (6S,9R)-6-(2,3-difluorophenyl)-3-(2-oxoethyl)-6,7,8,9-tetrahydro-5H-imidazo[1,2-a]azepin-9-ylcarbamate (85 mg, 0.210 mmol) in tetrahydrofuran (5 mL). After 2 h, the reaction was quenched with saturated aqueous ammonium chloride. Saturated aqueous sodium bicarbonate was added and the mixture was extracted with dichloromethane (3×). The combined organic extracts were dried over sodium sulfate, filtered, and concentrated. Purification by silica gel chromatography (100% dichloromethane→95% dichloromethane/methanol) gave the title compound (73 mg). MS 422.2 (M+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08039460B2 |
| Source dataset | uspto-grants-2011_10 |
| ORD ID | ord-2642321c83fd49b3b37254e1f713d24f |
| Source note | uspto-grants-2011_10 |