Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | Ethane, 1-fluoro-2-iodo- | HCID 69804 | — |
| Reactant | HCID 15908875 | HCID 15908875 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 22632943 | HCID 22632943 | 65.1% |
Reaction Steps
A solution of 3-benzyloxy-6,7-difluoro-1H-quinazoline-2,4-dione (Example B, 1.0 g, 3.2 mmol) in 20 mL of DMF was added to a suspension of sodium hydride (0.16 g, 3.9 mmol) in 20 mL of DMF and stirred for 30 minutes. 2-Fluoroethyl iodide (1.1 g, 6.4 mmol) was added, and the mixture was warmed to 50° C. for 18 hours. The reaction was quenched with 1 mL of water and concentrated to an oil. The residue was dissolved in chloroform, washed with water, brine and dried over magnesium sulfate. The solution was concentrated to give 0.73 g of the title compound as a solid, mp 145-147° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06331538B1 |
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| Source dataset | uspto-grants-2001_12 |
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| ORD ID | ord-6a3750ad5fb24326a3935abde6c2bb00 |
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| Source note | uspto-grants-2001_12 |
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