Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ethylamine | HCID 6341 | — |
| Reactant | 7-Chloro-6-nitroquinazolin-4(1H)-one | HCID 135687504 | — |
| Solvent | 1-Butanol | HCID 263 | — |
| Product | HCID 135430303 | HCID 135430303 | 40% |
Reaction Steps
7-Chloro-6-nitro-4(3H)-quinazolinone (20.0 g, 88.7 mmol) was suspended in n-butanol (150 ml), 70% aqueous ethylamine solution (120 ml) was added thereto, and the mixture was stirred for 15 minutes to give a clear solution which was then heated for 9 hours in a sealed tube in an oil bath (oil bath temperature set at 100° C. ). After the reaction was completed, the reaction mixture was left and cooled to precipitate yellow solids (first crystal) which were then filtered off. The first crystal was washed with methanol and ether and dried to give the desired title compound (8.27 g, 40%). The filtrate obtained at the time of acquisition of the first crystal was concentrated to precipitate crystal which was then filtered off and subjected to the same procedures as above to give second crystal as the desired title compound (5.84 g, 24%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06127541 |
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| Source dataset | uspto-grants-2000_10 |
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| ORD ID | ord-7b17d115c4314ff5985f2092566ec707 |
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| Source note | uspto-grants-2000_10 |
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