HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dichloromethane → HCID 118075456, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | HCID 118076294 | HCID 118076294 | — |
| Product | HCID 118075456 | HCID 118075456 | 89% |
Reaction Steps
Trifluoroacetic acid (70 mL) was added to a solution of tert-butyl 5-cyclobutoxy-2,3-difluorophenylcarbamate (32 g, 107 mmol) in dichloromethane (320 mL), and the resulting solution stirred overnight at room temperature. The reaction solution was concentrated, and the residue was dissolved in dichloromethane (500 mL). A solution of HCl (4 M in 1,4-dioxane, 120 mL) was slowly added with stirring. The resulting mixture was concentrated and poured into ethyl ether (480 mL). The resulting precipitate was filtered, and the filter cake was dried under reduced pressure to afford 5-cyclobutoxy-2,3-difluoroaniline hydrogen chloride (21 g, 89%) as a light yellow solid. MS (ESI, pos. ion) m/z 200 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09388161B2 |
| Source dataset | uspto-grants-2016_07 |
| ORD ID | ord-427f00a84ac044508f1b3e42300ef34b |
| Source note | uspto-grants-2016_07 |