HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl Acetate → 2-Chloro-4-nitro-6-(trifluoromethyl)aniline
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | Chlorosuccinimide | HCID 31398 | — |
| Reactant | 4-Nitro-alpha,alpha,alpha-trifluoro-o-toluidine | HCID 67128 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | 2-Chloro-4-nitro-6-(trifluoromethyl)aniline | HCID 13784427 | 75% |
Reaction Conditions
| Temperature | 150 °C |
|---|
Reaction Steps
4-Nitro-2-trifluoromethyl-phenylamine (5.6 g) and N-chlorosuccinimide (4.0 g) were suspended in acetonitrile (15 mL) and heated to 150° C. for 10 minutes in a sealed microwave process vial. Ethyl acetate (80 mL) was added and the organic phase was washed with 5% aqueous NaOH (2×50 mL), water (2×50 mL) and brine (2×50 mL). The organic phase was dried over magnesium sulfate and concentrated in vacuo. The crude product was purified by flash chromatography to furnish 4.9 g (75% yield) of the title compound as a yellow solid. 1H NMR (500 MHz, CDCl3): 5.35 (b, 2H), 8.35 (b, 1H), 8.37 (b, 1H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07501414B2 |
| Source dataset | uspto-grants-2009_03 |
| ORD ID | ord-65064098cc944640a30038fea2b7af32 |
| Source note | uspto-grants-2009_03 |