HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 22632906, compound → HCID 9948030, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 22632906 | HCID 22632906 | — |
| Reactant | HCID 178418361 | HCID 178418361 | — |
| Catalyst | Pd barium sulfate | HCID 16218511 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 9948030 | HCID 9948030 | 99.2% |
Reaction Steps
Five percent Pd/BaSO4 (60 mg) was added to a solution of 3-benzyloxy-1-ethyl-6-fluoro-7-pyrrolidinyl-1H-quinazoline-2,4-dione (Example E, 0.21 g, 0.55 mmol) in 16 mL of THF. The mixture was shaken under 50 PSI of hydrogen for 31 hours, filtered, and concentrated to afford 0.16 g of a solid. This solid was dissolved in 1N sodium hydroxide and washed with chloroform. The chloroform layer was back extracted with sodium hydroxide, and the combined basic extracts were acidified to pH 3. The aqueous layer was extracted with chloroform, dried over magnesium sulfate, and concentrated to give 0.11 g of the title compound as a solid, mp 170-171° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06331538B1 |
| Source dataset | uspto-grants-2001_12 |
| ORD ID | ord-3e202dcdb95047cd859c351bcd19d46d |
| Source note | uspto-grants-2001_12 |