化工社化工社 化学情報印刷レポート · 研究参考用
Tetrahydrofuran → 6-chloro-3-methylspiro[1H-quinazoline-4,5'-imidazolidine]-2,2',4'-trione
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | S-Ethylisothiuronium bromide | HCID 200213 | — |
| 反応物 | HCID 14229949 | HCID 14229949 | — |
| 生成物 | 6-chloro-3-methylspiro[1H-quinazoline-4,5'-imidazolidine]-2,2',4'-trione | HCID 14229968 | 53.1% |
反応手順
5-Chloro-1-methylcarbamoylisatin (4.0 g) is dissolved in tetrahydrofuran (40 ml) and thereto are added 2-ethylisothiourea hydrobromide (4.0 g) and triethylamine (3.0 ml), and the mixture is stirred at room temperature for one hour. The reaction mixture is concentrated under reduced pressure to remove the solvent. To the residue [i.e. 6-chloro- 3-methyl-4-hydroxy-4-(2-ethylisothioureido)carbonyl-2-oxo-1,2,3,4-tetrahydroquinazoline] is added 10% hydrochloric acid (50 ml), and the mixture is stirred at 70°-80° C. for 3 hours. After cooling, the precipitates are taken by filtration to give 6-chloro-3-methyl-spiro[1,2,3,4-tetrahydroquinazoline-4,4'-imidazolidine]-2,2',5'-trione (2.5 g, yield 53.1%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04762839 |
| 出典データセット | uspto-grants-1988_08 |
| ORD ID | ord-850eaaccdc6e40e698af6ee15b322d76 |
| 出典メモ | uspto-grants-1988_08 |