HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 58024763, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 1,4-Dioxane | HCID 31275 | — |
| Reactant | HCID 58024775 | HCID 58024775 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 58024763 | HCID 58024763 | 99.3% |
Reaction Steps
To a solution of 1,1-dimethylethyl 4-[(8-bromooctanoyl)amino]benzoate (0.61 g, 1.5 mmol, as prepared in Intermediate 35) in dichloromethane (2 ml) was added a 4M solution of HCl in 1,4-dioxane (4 ml, about 10 equivalents), and the mixture was left to stand at ambient temperature for 18 hours. The mixture was evaporated to dryness and the residue was co-evaporated with dichloromethane (20 ml) to give the title compound as a white solid (0.51 g). LCMS showed MH+=342/344 (Br isotope pattern); TRET=3.34 min. NMR (d6-DMSO) suggested that the material was again about 75% pure and that the impurity from the previous reaction (Intermediate 35) was still present. The mixture was used without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08003663B2 |
| Source dataset | uspto-grants-2011_08 |
| ORD ID | ord-4681d52437bd4c96a3ba6dd57ceabae3 |
| Source note | uspto-grants-2011_08 |