HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonium iodide → HCID 58423949, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonium iodide | HCID 25487 | — |
| Reactant | HCID 58424217 | HCID 58424217 | — |
| Solvent | Ethanol, reaction products with ammonia, distn. residues | HCID 22020343 | — |
| Product | HCID 58423949 | HCID 58423949 | 18% |
Reaction Steps
A solution of 6-bromo-1′,2-dimethyl-2′-(methylthio)-2-phenylspiro[chroman-4,4′-imidazol]-5′(1′H)-one (292 mg, 0.667 mmol), NH4I (245.7 mg, 1.668 mmol) in a solution of NH3/EtOH (30 mL, 5 N) was heated at 110° C. in a CEM tube in a microwave reactor for 4 h. After cooling, the mixture was concentrated in vacuum to give the residue, which was purified by preparative TLC to afford 2′-amino-6-bromo-1′,2-dimethyl-2-phenylspiro [chroman-4,4′-imidazol]-5′(1′H)-one (45 mg, 18%). 1H-NMR (MeOD): 1.63 (s, 3H), 1.77 (s, 3H), 2.74 (d, 2H), 6.75 (d, 1H), 7.06 (d, 1H), 7.22 (m, 1H), 7.31 (m, 3H), 7.45 (m, 2H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08450308B2 |
| Source dataset | uspto-grants-2013_05 |
| ORD ID | ord-d7cd7e50997148d0b472175f51b97c71 |
| Source note | uspto-grants-2013_05 |