Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | HCID 135767899 | HCID 135767899 | — |
| Catalyst | Iron | HCID 23925 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Water | HCID 962 | — |
| Product | 1013117-35-5 | HCID 136013872 | 100.7% |
Reaction Steps
To a suspension of 6-chloro-7-nitroquinazoline-4-one (7.5 g, 33 mmol) in MeOH (250 mL) was added NH4Cl (17.7 g, 0.33 mol) dissolved in water (75 mL). Iron powder (18.5 g, 330 mmol) was added and the suspension was heated at 65° C. for 2 h. The warm reaction mixture was filtered over diatomaceous earth and washed several times with THF (1 L) and methanol (500 mL). The filtrate was concentrated, washed with water and dried under vacuum at 50° C. to afford the title compound (6.5 g, 90%) as a brown solid. ESI-MS m/z 196 [C8H6ClN3O+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08809326B2 |
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| Source dataset | uspto-grants-2014_08 |
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| ORD ID | ord-a111bca80fd34374af0fd0545523b698 |
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| Source note | uspto-grants-2014_08 |
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