HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 46195744, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Sodium Iodide | HCID 5238 | — |
| Reactant | HCID 66726559 | HCID 66726559 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 46195744 | HCID 46195744 | 61% |
Reaction Steps
To a solution of the product of Step A (0.0346 g; 0.0743 mmol) and NaI (0.033 g; 0.22 mmol) in anhydrous CH3CN (1 ml) Me3SiCl (0.1 ml) was added at room temperature under N2. After stirring for 30 min at room temperature MeOH (2 ml) was added and the resulting mixture was evaporated to dryness under reduced pressure. The residue was partitioned between EtOAc (5 ml) and 1% NaHCO3 (5 ml). The precipitate formed was filtered off, washed with H2O (5 ml), fresh EtOAc (5 ml) and dried to give the title compound (0.019 g; 61%) as creamy solid. 1H-NMR (DMSO-d6) 1.28-1.41 (m, 6H): 3.2-3.4 (m, 2H+H2O); 3.5-4.02 (m, 7H); 4.07-4.18 (m, 4H); 4.6 (broad s, 2H); 6.52 (d, 1H, J=6 Hz); 7.06-7.19 (m, 3H); 7.58 (d, 1H, J=3 Hz); 7.72 (dd, 1H, J=9 Hz).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09181182B2 |
| Source dataset | uspto-grants-2015_11 |
| ORD ID | ord-310346c53c6745c485942444949a26ac |
| Source note | uspto-grants-2015_11 |