HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dichloromethane → 2-Cyclopropyl-7-iodo-1-benzofuran-5-amine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | 2-Cyclopropyl-7-iodo-5-nitrobenzofuran | HCID 118021828 | — |
| Catalyst | Iron | HCID 23925 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | 2-Cyclopropyl-7-iodo-1-benzofuran-5-amine | HCID 118022219 | 83.6% |
Reaction Steps
To a solution of the title compound from Step 1 (2.0 g, 6.0 mmol) and Fe (1.0 g, 18 mmol) in MeOH (80 mL) was added sat. NH4Cl solution (10 mL). The reaction mixture was refluxed for 1 h. The mixture was cooled to room temperature and poured into 400 mL of DCM. The resulting mixture was filtered and the filtrate was washed with water (100 mL) and brine. The organic layer was dried over anhydrous Na2SO4, filtered and concentrated under reduced pressure to give the crude title compound (1.5 g, 83% yield) as red oil that was used for the next step directly. 1H NMR (CDCl3, 400 MHz): δ 6.87 (d, J=2.4 Hz, 1H), 6.61 (d, J=2.0 Hz, 1H), 6.19 (s, 1H), 3.45 (br, 2H), 1.97-1.90 (m, 1H), 0.95-0.85 (m, 4H). LCMS: 300 (M+1)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09034900B2 |
| Source dataset | uspto-grants-2015_05 |
| ORD ID | ord-ef2f54e553c2425197dd499286f5d804 |
| Source note | uspto-grants-2015_05 |