HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Nitrite → Quinazoline-4,7-diol
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Nitrite | HCID 23668193 | — |
| Reactant | 7-Amino-quinazolin-4-ol | HCID 135478031 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Sulfuric acid hydrate (1:1) | HCID 21910475 | — |
| Product | Quinazoline-4,7-diol | HCID 135451644 | 76% |
Reaction Steps
A solution of sodium nitrite (1.40 g, 20.32 mmol) in water (17 mL) was added dropwise to a cooled suspension of 7-aminoquinazolin-4-one (712 mg, 4.42 mmol) in sulfuric acid/water (4.4 mL, 18 mL), keeping the temperature at approx. 0° C. The mixture was stirred at room temperature for 2 hours, diluted with water (15 mL) and heated at reflux for 15 minutes. The cooled mixture was neutralized and the precipitate was collected via filtration, and purified by column chromatography (silica) using 10% methanol/ethyl acetate as the eluent. The combined fractions gave an orange solid (541 mg, 76%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08624025B2 |
| Source dataset | uspto-grants-2014_01 |
| ORD ID | ord-805c4706127f404588a3d27dab069af9 |
| Source note | uspto-grants-2014_01 |