HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethanol → 4-(3-Aminophenyl)-6,7-dimethoxy-2-methylaminoquinazoline
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethanol | HCID 702 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | HCID 12150401 | HCID 12150401 | — |
| Reactant | HCID 178418361 | HCID 178418361 | — |
| Catalyst | HCID 178418390 | HCID 178418390 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 4-(3-Aminophenyl)-6,7-dimethoxy-2-methylaminoquinazoline | HCID 15540531 | 73.1% |
Reaction Steps
1.83 g of 6,7-dimethoxy-2-methylamino-4-(3-nitrophenyl) quinazoline obtained in Production Example 4,200 mg of 10% palladium-carbon powder (hydrate) and 1.44 g triethylamine were suspended in a mixed solvent of 10 ml ethanol and 10 ml tetrahydrofuran. After the atmosphere was replaced with hydrogen, the mixture was stirred for 15 hours at ordinary pressure at room temperature. The reaction solution was filtered, then the filtrate was evaporated, and the crude product was purified and separated by silica gel column chromatography (hexane:ethyl acetate=1:3). The product was recrystallized from hexane-ethyl acetate to give 1.22 g of the title compound as pale yellow crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06352989B1 |
| Source dataset | uspto-grants-2002_03 |
| ORD ID | ord-00bcdbf9eef048c8985e26b5df30abbc |
| Source note | uspto-grants-2002_03 |