HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lithium Hydroxide → HCID 136248868, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lithium Hydroxide | HCID 3939 | — |
| Reactant | 5-(Benzyloxy)-2-methoxybenzaldehyde | HCID 10966694 | — |
| Reactant | HCID 136248856 | HCID 136248856 | — |
| Solvent | 15-Crown-5 | HCID 36336 | — |
| Product | HCID 136248868 | HCID 136248868 | 18.2% |
Reaction Conditions
| Temperature | 100 °C |
|---|
Reaction Steps
A mixture of 2-(6-bromopyridin-2-yl)-5,7-dimethoxyquinazolin-4(3H)-one (5 Scheme 21, 0.100 g, 0.278 mmol), 1-methylpiperazin-2-one (7, 0.100 g, 0.667 mmol) and anhydrous lithium hydroxide (0.020 g, 0.83 mmol) in 15-crown-5 (0.9 mL) was heated at 100° C. for 18 h. The mixture was cooled to room temperature and purified by reverse phase HPLC eluting with 10% to 90% CH3CN in H2O to afford the title compound (0.02 g, 18%) as an off-white solid: 1H NMR (500 MHz, DMSO-d6) δ 11.33 (s, 1H), 7.78 (t, J=7.5 Hz, 1H), 7.73 (d, J=7.1 Hz, 1H), 7.08 (d, J=8.3 Hz, 1H), 6.78 (d, J=2.2 Hz, 1H), 6.58 (d, J=2.2 Hz, 1H), 4.25 (s, 2H), 3.97 (t, J=5.5 Hz, 2H), 3.91 (s, 3H), 3.87 (s, 3H), 3.47 (t, J=5.3 Hz, 2H), 2.93 (s, 3H); ESI MS m/z 396 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09073878B2 |
| Source dataset | uspto-grants-2015_07 |
| ORD ID | ord-3d69eba8dbb240cfb3c66e0d784c12d2 |
| Source note | uspto-grants-2015_07 |