HuagongsheHuagongshe Chemistry Print Report · For research reference only
N-Iodosuccinimide → HCID 68839933, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | N-Iodosuccinimide | HCID 120273 | — |
| Reactant | HCID 57932986 | HCID 57932986 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 68839933 | HCID 68839933 | 88% |
Reaction Steps
To a solution of 8-(1-ethyl-propyl)-3-(3-methoxy-thiophen-2-yl)-2,6-dimethyl-imidazo[1,2-b]pyridazine (0.75 g, 2.28 mmol) and CH3CN (10 mL) is added NIS (0.54 g, 2.39 mmol). The solution is stirred overnight, concentrated, diluted with EtOAc (30 mL), washed with water (30 mL), sat. NH4Cl (30 mL), 20% (NaHSO3) (30 mL), brine (30 mL), dried over MgSO4, filtered and concentrated. The residue is purified by ISCO column chromatography (15%-20% EtOAc/hexane gradient) furnish the title compound (0.91 g, 2.00 mmol, 88%). 1H NMR (CDCl3) δ 0.85 (t, J=7.5 Hz, 6H), 1.71-1.89 (m, 4H), 2.46 (s, 3H), 2.52 (s, 3H), 3.25-3.35 (m, 1H), 3.83 (s, 3H), 6.64 (s, 1H), 7.12 (s, 1H). LC/MS (m/z): calcd. for C18H22IN3OS (M+H)+: 456.4; found: 456.0.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07612067B2 |
| Source dataset | uspto-grants-2009_11 |
| ORD ID | ord-70cd8e4ded6b45729caca18bc5a46bb0 |
| Source note | uspto-grants-2009_11 |