HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonium iodide → HCID 58424154, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonium iodide | HCID 25487 | — |
| Reactant | HCID 58424303 | HCID 58424303 | — |
| Solvent | Ethanol, reaction products with ammonia, distn. residues | HCID 22020343 | — |
| Product | HCID 58424154 | HCID 58424154 | 50% |
Reaction Steps
A solution of 6-bromo-2-(3-fluorophenyl)-1′-methyl-2′-(methylthio)spiro[chroman-4,4′-imidazol]-5′(1′H)-one (80 mg, 0.18 mmol) and NH4I (52 mg, 0.36 mmol) in NH3/EtOH (4 mL, 1.5 N) was heated at 110° C. in a tube in a microwave reactor for 2-2.5 h. After cooling, the mixture was concentrated in vacuo to give a residue, which was purified by preparative TLC and then by preparative HPLC to afford 2′-amino-6-bromo-2-(3-fluorophenyl)-1′-methylspiro[chroman-4,4′-imidazol]-5′(1′H)-one (36 mg, 50%). 1H-NMR (MeOD): 2.16 (m, 2H), 3.12 (s, 3H), 5.87 (d, 1H), 6.90 (d, 1H), 7.08 (m, 2H), 7.25 (m, 2H), 7.33 (d, 1H), 7.41 (m, 1H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08450308B2 |
| Source dataset | uspto-grants-2013_05 |
| ORD ID | ord-adf5347b3bf34094a403d648a1a676e3 |
| Source note | uspto-grants-2013_05 |