HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrogen Peroxide → HCID 59729943, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrogen Peroxide | HCID 784 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | HCID 59730056 | HCID 59730056 | — |
| Solvent | Dimethyl Sulfoxide | HCID 679 | — |
| Product | HCID 59729943 | HCID 59729943 | 96.8% |
Reaction Steps
Combine nitrile, 6-[4-(2-benzylamino-ethyl)-2-methyl-phenoxy]-nicotinonitrile (compound of example 219, step 3) (13 mg, 0.04 mmol), H2O2 (5 μL) and K2CO3 (3 mg, 0.02 mmol) in DMSO (0.2 mL), and stir the mixture at room temperature overnight. Add water and extract the aqueous layer with EtOAc. Dry the organic layer over Na2SO4 and eliminate the solvent. Purify by flash chromatography (eluent: CHCl3/0.5% EtOH/0.05% NH4OH) to give the title compound (7 mg, 52%). Electrospray MS M+1 ion=362. 1H-NMR (methanol-d4, 300 MHz): 8.59 (d, 1H, J=2.5 Hz), 8.24 (dd, 1H, J=2.5 and 8.0 Hz), 7.33-7.21 (m, 5H), 7.15-7.07 (m, 2H), 6.98-6.93 (m, 2H), 3.78 (s, 2H), 2.83 (s, 4H), 2.09 (s, 3H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07560463B2 |
| Source dataset | uspto-grants-2009_07 |
| ORD ID | ord-c72e64626eb7481abe5f89aafdce4f5b |
| Source note | uspto-grants-2009_07 |