HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 76831217, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 76831279 | HCID 76831279 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 76831217 | HCID 76831217 | 255% |
Reaction Steps
Crude (1SR,7RS)-1-[5-(benzhydrylidene-amino)-2-fluoro-phenyl]-5-oxa-2-aza-bicyclo[5.1.0]octane-3-thione (intermediate B12A) (600 mg, 1.15 mmol) was dissolved in dioxane (15 ml) and 1 M HCl (1.44 ml, 1.44 mmol) was added at 23° C. After 30 min of stirring, the reaction mixture was poured on sat. NaHCO3-solution and extracted twice with ethyl acetate. The combined organic layers were washed with brine, dried over sodium sulfate, filtered and evaporated to give a dark green oil (740 mg), which was purified by silica gel column chromatography with dichloromethane/ethyl acetate to give the title compound as a light yellow solid (175 mg, 60%). MS (ISP): m/z=253.2 [(M+H)+].
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08673894B2 |
| Source dataset | uspto-grants-2014_03 |
| ORD ID | ord-4e21d595d5594d0ab0171c6238b418e2 |
| Source note | uspto-grants-2014_03 |