HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethanol → HCID 22663125, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethanol | HCID 702 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | HCID 12150252 | HCID 12150252 | — |
| Reactant | HCID 178418361 | HCID 178418361 | — |
| Catalyst | Lindlars catalyst | HCID 131709914 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 22663125 | HCID 22663125 | 63.6% |
Reaction Steps
70.0 mg of 6,7-dimethoxy-2-methylamino-4-[3-(2-phenyl ethynyl)phenyl]quinazoline obtained in Example 65, 50.0 mg Lindlar catalyst and 50.0 mg triethylamine were suspended in a mixed solvent of 5 ml ethanol and 5 ml tetrahydrofuran. After the atmosphere was replaced with hydrogen, the mixture was stirred for 6 hours at ordinary pressure at room temperature. The reaction solution was filtered, and the filtrate was evaporated. Then, the crude product was purified and separated by silica gel column chromatography (hexane:ethyl acetate=2:1). The product was recrystallized from hexane-isopropanol to give 45.0 mg of the title compound as colorless crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06800644B2 |
| Source dataset | uspto-grants-2004_10 |
| ORD ID | ord-addd63bfcb004d50b0a28c873e8379c3 |
| Source note | uspto-grants-2004_10 |