Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Diethyl (ethoxymethylene)malonate | HCID 6871 | — |
| Reactant | HCID 13060449 | HCID 13060449 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Chloroform methanol | HCID 21584188 | — |
| Product | HCID 13060567 | HCID 13060567 | 18.4% |
Reaction Steps
A mixture of 4-amino-6,7-dimethylquinazoline (11.3 g) and diethyl ethoxymethylenepropanedioate (15.55 g) in N,N-dimethylformamide (45 ml) was stirred for 4 hours at 110° C. After the reaction mixture was cooled to ambient temperature, to the mixture was added water to give crystals, which were separated by filtration, washed with water and dried under reduced pressure to give crude crystals (18.5 g). The crude crustals were dissolved in 1% methanol-chloroform solution (500 ml) and concentrated under reduced pressure after insoluble materials were removed by filtration. The residue was recrystallized from chloroform to give crystalline ethyl 9,10-dimethyl-4-oxo-4H-pyrimido[1,2-c]quinazoline-3-carboxylate (3.57 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04377580 |
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| Source dataset | uspto-grants-1983_03 |
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| ORD ID | ord-95ccd14415184ecd9738dc45081aab77 |
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| Source note | uspto-grants-1983_03 |
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