HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 3-(1,1-Difluoroethyl)aniline
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Ethanol | HCID 702 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 13412531 | HCID 13412531 | — |
| Catalyst | Iron | HCID 23925 | — |
| Product | 3-(1,1-Difluoroethyl)aniline | HCID 23445092 | — |
Reaction Steps
Dissolve the nitro compound obtained in Step 1 (870 mg, 4.8 mmol) in ethanol (10 mL), add iron powder (1.3 g, 23.3 mmol), concentrated aqueous HCl (37%, 2.7 mL), stir the reaction at room temperature for 2 hrs. After the reaction, carefully neutralize the mixture with NaOH solution. Filter off the solid, pour the filtrate to ice water (50 mL), extract with EtOAc (15 mL×3), combine the organic layers, wash with brine (100 mL) and dry over anhydrous Na2SO4. Concentrate under reduced pressure to get the crude product (760 mg) which is used without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09359338B2 |
| Source dataset | uspto-grants-2016_06 |
| ORD ID | ord-69648884d92b42efab6f2e9652217f5f |
| Source note | uspto-grants-2016_06 |