HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl Acetate → 3,5-Dichloro-4-(2,2,2-trifluoroethoxy)aniline
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Stannous Chloride | HCID 24479 | — |
| Reactant | 1,3-Dichloro-5-nitro-2-(2,2,2-trifluoroethoxy)benzene | HCID 13852227 | — |
| Solvent | Hydrochloric Acid | HCID 313 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | 3,5-Dichloro-4-(2,2,2-trifluoroethoxy)aniline | HCID 13852146 | 94% |
Reaction Steps
To a solution of 1,3-dichloro-5-nitro-2-(2,2,2-trifluoroethoxy)benzene (1.90 g, 6.55 mmol) in MeOH (20 mL) and 12 N HCl (20 mL) at rt, SnCl2 (3.72 g, 19.66 mmol) was slowly added to it and then the reaction mixture was stirred overnight at rt. To the reaction mixture was slowly added 3N NaOH to pH=10 and then extracted with EA. The combined organic layers were washed with brine, dried over anhydrous Na2SO4, and concentrated under reduced pressure. The residue was purified by column chromatography over silica gel eluted with PE:EA (6:1) to provide 3,5-dichloro-4-(2,2,2-trifluoroethoxy)aniline (1.60 g, yield 94%) as pale yellow oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08853186B2 |
| Source dataset | uspto-grants-2014_10 |
| ORD ID | ord-ae1e0c4f0cb74bbb84f8d051cd35e0bd |
| Source note | uspto-grants-2014_10 |