HuagongsheHuagongshe Chemistry Print Report · For research reference only
Imidazole → (R)-4-(3-Iodo-2-methylpropyl]-4H-benzo[1,4]oxazin-3-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Imidazole | HCID 795 | — |
| Reactant | Iodine | HCID 807 | — |
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | (R)-4-(3-Hydroxy-2-methylpropyl]-4H-benzo[1,4]oxazin-3-one | HCID 68910321 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | (R)-4-(3-Iodo-2-methylpropyl]-4H-benzo[1,4]oxazin-3-one | HCID 68908541 | 87.4% |
Reaction Steps
A reaction flask was charged with (R)-4-(3-Hydroxy-2-methylpropyl]-4H-benzo[1,4]oxazin-3-one (1.71 g, 7.77 mmol), triphenylphosphine (4.50 g, 17.2 mmol), imidazole (1.27, 18.7 mmol), and iodine (5.54 g, 21.8 mmol) in CH2Cl2 (20 mL) and stirred at rt for 20 h. The reaction mixture was washed with saturated sodium thiosulfate, dried over Na2SO4, filtered, and concentrated. The product was purified by flash column chromatography (SiO2; n-heptane/EtOAc 2:1) to give the title compound (2.25 g, 87%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07550459B2 |
| Source dataset | uspto-grants-2009_06 |
| ORD ID | ord-a0c60ea4c2da480d97f088b1054e8e8d |
| Source note | uspto-grants-2009_06 |