関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Diphenyl Ether | HCID 7583 | — |
| 反応物 | Dimethyl[[6-(2-ethylbutyramido)-4-quinazolinylamino]methylene]propanedioate | HCID 13060503 | — |
| 溶媒 | Hexane | HCID 8058 | — |
| 生成物 | methyl 4-oxo-10-(2-ethylbutyramido)-4H-pyrimido[1,2-C]quinazoline-3-carboxylate | HCID 13060555 | 78.1% |
反応手順
A mixture of dimethyl[[6-(2-ethylbutyramido)-4-quinazolinylamino]methylene]propanedioate (5.3 g) and diphenyl ether (32 ml) was heated at 255° C. for 15 minutes and cooled to ambient temperature. Hexane was added to the reaction mixture. The resulting crystals were filtered off, washed with hexane and dried. The crude crystals were dissolved in a mixture of chloroform and methanol (10:1) under heating. Insoluble materials were removed by filtration. The filtrate was concentrated under reduced pressure to give crystals, which were recrystallized from a mixture of chloroform and hexane to give methyl 4-oxo-10-(2-ethylbutyramido)-4H-pyrimido[1,2-C]quinazoline-3-carboxylate (3.81 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US04377580 |
|---|
| 出典データセット | uspto-grants-1983_03 |
|---|
| ORD ID | ord-c2457fe689d94c68b6796249a04d2da1 |
|---|
| 出典メモ | uspto-grants-1983_03 |
|---|