HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetyl chloride → HCID 59722689, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetyl chloride | HCID 6367 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 59722595 | HCID 59722595 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 59722689 | HCID 59722689 | 82.8% |
Reaction Steps
Acetyl chloride (24 μL, 0.344 mmol) was added to a solution of tert-butyl (6S,9R)-6-(2,3-difluorophenyl)-3-(2-hydroxyethyl)-6,7,8,9-tetrahydro-5H-imidazo[1,2-a]azepin-9-ylcarbamate (70 mg, 0.172 mmol) and triethylamine (48 μL, 0.344 mmol) in dichloromethane (6 mL) at 0° C. After 1.5 h, saturated aqueous sodium bicarbonate was added and the mixture was extracted with dichloromethane (2×). The combined organic extracts were dried over magnesium sulfate, filtered, and concentrated. Purification by silica gel chromatography (100% dichloromethane→95% dichloromethane/methanol) gave the title compound (64 mg). MS 450.2 (M+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08039460B2 |
| Source dataset | uspto-grants-2011_10 |
| ORD ID | ord-46655f19fba340ce974f2c6213e87c68 |
| Source note | uspto-grants-2011_10 |