HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 2-Chloro-4-methoxyaniline
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 4-Bromo-2-chloroaniline | HCID 610169 | — |
| Reactant | Sodium Methoxide | HCID 10942334 | — |
| Catalyst | Copper iodide | HCID 83717 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | 2-Chloro-4-methoxyaniline | HCID 407432 | 41% |
Reaction Steps
A mixture of 4-bromo-2-chloro-aniline (25.0 g, 121 mmol), copper iodide (23.1 g, 121 mmol), and a solution of sodium methoxide in methanol (28%, 125 mL) was stirred for 1 h at 100° C. The reaction mixture was poured into a mixture of hydrochloric acid (6 M, 100 mL) and ice, and washed with ethyl acetate. The aqueous phase was basified with aqueous sodium hydroxide (8 M) and extracted with ethyl acetate. The extracts was washed with brine, dried over sodium sulfate, filtrated, and concentrated in vacuo. The residue was purified by column chromatography on silica gel eluting with a 30% ethyl acetate/n-hexane gradient mixture to give the title compound as a pale yellow oil (7.90 g, 50.1 mmol, 41%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08785460B2 |
| Source dataset | uspto-grants-2014_07 |
| ORD ID | ord-5162ac3db5174f008e476b2fe794d135 |
| Source note | uspto-grants-2014_07 |