HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 59722739, compound → HCID 59722606, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 59722739 | HCID 59722739 | — |
| Reactant | HCID 178418573 | HCID 178418573 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 59722606 | HCID 59722606 | 71.2% |
Reaction Steps
Methylmagnesium bromide (3.0 M in ether; 90 μL, 0.27 mmol) was added to a solution of tert-butyl (6S,9R)-3-acetyl-6-(2,3-difluorophenyl)-6,7,8,9-tetrahydro-5H-imidazo[1,2-a]azepin-9-ylcarbamate (22 mg, 0.05 mmol) in tetrahydrofuran (1 mL) at 0° C., and the reaction mixture was allowed to warm to ambient temperature. After 30 min, the reaction was quenched with water and the mixture was extracted with dichloromethane (3×). The organic layer was washed with water, saturated brine, dried over magnesium sulfate, filtered and concentrated. Purification by reverse phase HPLC (C-18, 95% water/acetonitrile→5% water/acetonitrile with 0.1% trifluoroacetic acid) gave the title compound (15 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-9430af1994304c8ba64c74b3c236cad3 |
| Source note | uspto-grants-2011_10 |