HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl Acetate → HCID 57786111, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | HCID 57785882 | HCID 57785882 | — |
| Reactant | HCID 178418630 | HCID 178418630 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 57786111 | HCID 57786111 | 65% |
Reaction Steps
To a stirred solution of [10-chloro-1-(2,4-dichlorophenyl)-4,5-dihydro-1H,3H-[1,4]oxazepino[4,3-a]benzimidazol-7-yl](cyclopropyl)methanone (67.1 mg, 0.154 mmol) in tetrahydrofuran (1 mL) was added a solution of cyclopropyl magnesium bromide in tetrahydrofuran (1.0 M, 4.62 mL, 4.62 mmol) at 0° C. After 15 min, the reaction mixture was poured into a mixture of ethyl acetate and aqueous ammonium chloride. The organic phase was washed with brine, dried over sodium sulfate, filtrated, and concentrated in vacuo. The residue was purified by flash column chromatography on NH silica gel eluting with a 0-25% ethyl acetate/n-hexane gradient mixture to give the title compound as a colorless solid (48.2 mg, 0.101 mmol, 65%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08901141B2 |
| Source dataset | uspto-grants-2014_12 |
| ORD ID | ord-9396e5f1b99d4fdeab27f8afae1f442c |
| Source note | uspto-grants-2014_12 |