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Tetrahydrofuran → 1(m-nitrophenyl)-3-allylquinazoline-2,4(1H, 3H)-dione
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | Phosgen toluene | HCID 19083224 | — |
| 反応物 | 2-(m-nitroanilino)-N-allylbenzamide | HCID 21444004 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1(m-nitrophenyl)-3-allylquinazoline-2,4(1H, 3H)-dione | HCID 13272344 | — |
反応手順
To a solution of 3.0 g of 2-(m-nitroanilino)-N-allylbenzamide and 25 ml of tetrahydrofuran was added 1.1 g of 50 % sodium hydride, and the whole was stirred for 30 minutes at room temperature. To this was added dropwise under cooling 16 g of 30 % phosgene-toluene solution, and the mixture was stirred for one hour at room temperature and then refluxed for 2 hours. After the reaction was finished, the solvent was distilled off from the resulting mixture, and to the residue obtained was added water to precipitate a crude product. This product was recrystallized from methanol to yield 2.8 g of 1-(m-nitrophenyl)-3-allylquinazoline-2,4(1H, 3H)-dione as colorless needles, melting at 164°-166° 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-275e0f4243df42678651f6d289c93cb3 |
| 出典メモ | uspto-grants-1977_04 |