HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 86726414, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | HCID 86726415 | HCID 86726415 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 86726414 | HCID 86726414 | 48% |
Reaction Steps
4M HCl (7.60 mL, 30.4 mmol) in dioxane was added to a solution of tert-butyl (3,6-difluoro-2-iodophenyl)carbamate (1.08 g, 3.04 mmol) in THF (7.60 ml) at room temperature and then stirred overnight. The solvent was removed in vacuo, and then the contents were partitioned between DCM (3×50 mL) and sat'd aqueous sodium bicarbonate. The organics were dried over MgSO4, filtered and concentrated. The crude material was purified on silica gel, eluting 0-50% EtOAc in hexanes over 16 minutes to afford 3,6-difluoro-2-iodoaniline (373 mg, 1.46 mmol) as a tan oil. MS (ESI): m/z=256.2 (M+H-Boc).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09315475B2 |
| Source dataset | uspto-grants-2016_04 |
| ORD ID | ord-efcbf90f21a6444f94f347465a246b0b |
| Source note | uspto-grants-2016_04 |