HuagongsheHuagongshe Chemistry Print Report · For research reference only
Carbamic acid, ethyl ester → HCID 136116269, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Carbamic acid, ethyl ester | HCID 5641 | — |
| Reactant | Phosphorus oxide (P4O10) | HCID 14812 | — |
| Reactant | Ethyl 4-[(2-methoxybenzoyl)amino]benzoate | HCID 1739885 | — |
| Solvent | O-Xylene | HCID 7237 | — |
| Product | HCID 136116269 | HCID 136116269 | 70.7% |
Reaction Steps
Ethyl 4-(2'-methoxy-benzoylamino)-benzoate (21 g), prepared according to Example 19 is reacted with ethyl carbamate (12 g) and P2O5 (70 g) in xylene (200 ml) for 6 hours at the reflux temperature. After cooling, the precipitate is filtered off, poured in ice-water and treated with NaOH to neutralization. The precipitate (23 g) is collected by filtering and is hydrolyzed by treatment with LiBr (10 moles/mole) in dimethylformamide (150 ml) at the reflux temperature for 2 hours. After cooling, acidify with acetic acid, filter and wash with hot ethanol to obtain 6-carboxy-2-(2'-methoxy-phenyl)-3,4-dihydro-4-oxo-quinazoline (14.7 g; m.p. 296°-297° C.).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04251531 |
| Source dataset | uspto-grants-1981_02 |
| ORD ID | ord-3bfc67c71477487ab87b6a903e777696 |
| Source note | uspto-grants-1981_02 |