HuagongsheHuagongshe Chemistry Print Report · For research reference only
Iodine → HCID 66753013, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Iodine | HCID 807 | — |
| Reactant | HCID 3161846 | HCID 3161846 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 66753013 | HCID 66753013 | — |
Reaction Steps
To a solution of Step 2 intermediate (1.2 g, 5.620 mmol) in acetonitrile (15 ml) was added ceric ammonium nitrate (1.53 g, 2.812 mmol) followed by iodine (0.857 g, 3.325 mmol) and refluxed for 2.0 h. After completion of the reaction, the solvent was evaporated and the residue dissolved in ethyl acetate. Combined organic layer was washed with water, saturated NaHSO3 solution, brine and dried and purified to afford the desired compound: 1H NMR (300 MHz, DMSO-d6) δ 2.61 (s, 3H), 3.75 (s, 3H), 7.39-7.42 (s, 1H), 7.52-7.58 (m, 1H), 7.68-7.70 (m, 1H), 8.38-8.41 (s, 1H); ESI-MS (m/z) 340.48 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08518955B2 |
| Source dataset | uspto-grants-2013_08 |
| ORD ID | ord-9928f251b97647958d675e606035f73f |
| Source note | uspto-grants-2013_08 |