HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,4-Dioxane → HCID 178505899, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,4-Dioxane | HCID 31275 | — |
| Reactant | HCID 178442166 | HCID 178442166 | — |
| Solvent | Hydrochloric Acid | HCID 313 | — |
| Solvent | Dimethyl sulfoxide methanol | HCID 22036561 | — |
| Product | HCID 178505899 | HCID 178505899 | 34.3% |
Reaction Steps
1,1-Dimethylethyl(trans-3-{[4-fluoro-3-(trifluoromethyl)phenyl]oxy}cyclobutyl)(imidazo[1,2-a]pyridin-8-ylmethyl)carbamate (62 mg, 0.129 mmol) was stirred in 4M HCl in dioxane (5 mL, 20 mmol) for 3 hours when LCMS indicated the reaction to be complete. The mixture was loaded onto a SCX cartridge (2 g) and eluted with MeOH (3 column volumes) and flushed with ammonia in MeOH. The eluant was concentrated in vacuo to give slightly impure product which was dissolved in 50:50 DMSO/MeOH (1 mL) and purified by MDAP to give the title compound (16.8 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08754101B2 |
| Source dataset | uspto-grants-2014_06 |
| ORD ID | ord-455da437546f477495530a823f32feb9 |
| Source note | uspto-grants-2014_06 |