HuagongsheHuagongshe Chemistry Print Report · For research reference only
Iodine → HCID 68801661, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Iodine | HCID 807 | — |
| Reactant | Bromine | HCID 24408 | — |
| Reactant | Phosphorus pentachloride | HCID 24819 | — |
| Reactant | HCID 68802665 | HCID 68802665 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 68801661 | HCID 68801661 | — |
Reaction Steps
Phosphorus pentachloride (0.3 g, 1.44 mmol) was added slowly to a solution of 1-(cyclopropylmethyl)-5-phenylazepan-2-one (0.35 g, 1.44 mmol) in dichloromethane (8 mL) at 0° C. After 1 h, iodine (3.6 mg, 0.01 mmol) and bromine (0.07 mL, 1.44 mmol) were added, and the mixture was allowed to warm to ambient temperature. After 1 h, another 0.3 g of phosphorus pentachloride was added. After an additional 18 h, the reaction was quenched with saturated sodium bicarbonate. The mixture was extracted with dichloromethane (3×), and the combined organic extracts were washed with water (3×), saturated brine, dried over sodium sulfate, filtered and concentrated.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07491713B2 |
| Source dataset | uspto-grants-2009_02 |
| ORD ID | ord-91a8cd1abb9c4020966644b7dd08fd9c |
| Source note | uspto-grants-2009_02 |