HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dichloromethane ethanol → HCID 6481660, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dichloromethane ethanol | HCID 21584144 | — |
| Reactant | Acetate-hydrochloric acid | HCID 22641269 | — |
| Reactant | HCID 59687010 | HCID 59687010 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 6481660 | HCID 6481660 | 71.2% |
Reaction Steps
Dried N-[(1S,1aR,7bR)-4,7-difluoro-1,1a,2,7b-tetrahydrocyclopropa[c]chromen-1-yl]-N′-[5-(4-(N-t-butoxycarbonylamino)phenoxy)-2-pyridinyl]urea (242 mg, 0.46 mmol) was dissolved in methylene chloride (2 ml) and then 1M HCl/AcOH (4.6 ml) was added and the reaction solution was stirred for 60 minutes at room temperature. The volatile matters were removed by evaporation. The residue was worked up by extractions between methylene chloride and sat. aq. NaHCO3. The organic phase was dried through sodium sulfate and evaporated. Silica gel column chromatography (1-3% EtOH/methylene chloride gradient) gave 139 mg of pure product as white powder (71% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07915295B2 |
| Source dataset | uspto-grants-2011_03 |
| ORD ID | ord-e88f969e163e449c993f629ad20c25b3 |
| Source note | uspto-grants-2011_03 |