化工社化工社 化学情報印刷レポート · 研究参考用
Dimethylformamide → 1-(m-nitrophenyl)-3-methylquinazoline-2,4(1H, 3H)-dione
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | Dimethyl sulfite | HCID 69223 | — |
| 反応物 | 1-(m-nitrophenyl)quinazoline-2,4(1H, 3H)-dione | HCID 12812377 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1-(m-nitrophenyl)-3-methylquinazoline-2,4(1H, 3H)-dione | HCID 12812378 | — |
反応手順
To a solution of 2.8 g of 1-(m-nitrophenyl)quinazoline-2,4(1H, 3H)-dione and 30 ml of dimethylformamide was added 0.6 g of approximately 55 % sodium hydride, and the solution was stirred for 20 minutes at room temperature. To this was added 2.2 g of dimethyl sulfite and stirring was further continued for 4 hours at room temperature. After the reaction was complete, the solvent was removed from the reaction mixture by distillation under reduced pressure. The residue thus obtained was mixed with water to precipitate a crude product. This product was recrystallized from methanol to afford 2.8 g of 1-(m-nitrophenyl)-3-methylquinazoline-2,4(1H, 3H)-dione as colorless needles, melting at 242°-243° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04016166 |
| 出典データセット | uspto-grants-1977_04 |
| ORD ID | ord-0c4cbc72e24d4188a445601834301607 |
| 出典メモ | uspto-grants-1977_04 |