HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dichloromethane → (4-Iodo-2,5-Dimethylphenyl)Amine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | 2,5-Dimethylaniline | HCID 7259 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | Tetramethylammonium Dichloroiodate | HCID 11737348 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Water | HCID 962 | — |
| Product | (4-Iodo-2,5-Dimethylphenyl)Amine | HCID 4770984 | 98% |
Reaction Steps
To a solution of 2,5-dimethylaniline (20 g, 165 mmol) in a 1:1 mixture of dichloromethane and methanol (400 mL) was added sodium bicarbonate (20.8 g, 250 mmol) and tetramethylammonium dichloroiodate(I) (44.7 g, 165 mmol). The resulting mixture was stirred at room temperature for 1 hour and then water was added (500 mL). The organic layer was removed and washed with 5% aqueous sodium thiosulfate (500 mL) and brine (500 mL). The organic layer was then dried over anhydrous magnesium sulfate, filtered and concentrated under vacuum to provide 4-iodo-2,5-dimethylphenylamine (39.6 g, 98% yield). The product was used without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08134006B2 |
| Source dataset | uspto-grants-2012_03 |
| ORD ID | ord-6ff240e4152f46de8e15740c903cc20d |
| Source note | uspto-grants-2012_03 |