HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 3-Chloro-2,6-difluoroaniline
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | tert-Butyl (3-chloro-2,6-difluorophenyl)carbamate | HCID 86083514 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | 3-Chloro-2,6-difluoroaniline | HCID 17750745 | 92.2% |
Reaction Steps
A solution of 1,1-dimethylethyl (3-chloro-2,6-difluorophenyl)carbamate (437 mg, 1.66 mmol) in methanol (2 mL) was treated with 4 N hydrochloric acid in dioxane (2 mL) and heated for 1 min with a heat gun. After cooling, the volatile materials were removed in vacuo. The resulting residue was taken up in ethyl acetate and washed with sodium bicarbonate (sat). The organic phase was dried over magnesium sulfate, filtered, and concentrated yielding 3-chloro-2,6-difluoroaniline as a white solid (250 mg, 1.53 mmol, 92%). MS (EI) for C6H4ClF2N: 164 (MH+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07846959B2 |
| Source dataset | uspto-grants-2010_12 |
| ORD ID | ord-831f157901ad4d4787c8a38d1b876075 |
| Source note | uspto-grants-2010_12 |