HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 178493687, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | Sodium Methoxide | HCID 10942334 | — |
| Reactant | 7-chloro-1H-pyrido[3,2-d]pyrimidin-4-one | HCID 178518219 | — |
| Product | HCID 178493687 | HCID 178493687 | — |
Reaction Steps
A microwave vial was charged with 7-chloropyrido[3,2-d]pyrimidin-4(1H)-one (110 mg, 0.606 mmol), a 0.5 M solution of sodium methoxide in methanol (3.65 mL, 1.817 mmol) and sodium methoxide (327 mg, 6.06 mmol). The vial was capped and irradiated in a microwave reactor at 145° C. for 30 minutes. The reaction was neutralized with saturated aqueous ammonium chloride (3 mL), concentrated, and diluted with cold water. The resulting precipitate was collected by vacuum filtration and dried in vacuo to provide the title compound (107 mg, 0.604 mmol) as pink solid. 1H NMR (400 MHz, DMSO-d6) δ ppm 3.95 (s, 3 H) 7.49 (d, J=2.74 Hz, 1 H) 8.11 (s, 1 H) 8.47 (d, J=2.74 Hz, 1 H). LC/MS (ESI+) m/z=178 (M+H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09296734B2 |
| Source dataset | uspto-grants-2016_03 |
| ORD ID | ord-aeda161efce34c1289ae93cf0a4107e2 |
| Source note | uspto-grants-2016_03 |