関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Allylamine | HCID 7853 | — |
| 反応物 | Cyanuric chloride | HCID 7954 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | N,N'-Diallyl-6-chloro-1,3,5-triazine-2,4-diamine | HCID 27306 | — |
反応手順
54.9 g (0.96 mole) of allylamine are added dropwise, in the course of 1.5 hours and while stirring, to a clear solution of 73.8 g (0.4 mole) of cyanuric chloride in 500 ml of toluene, the temperature being kept between 20° and 30° by applying gentle external cooling to the reaction vessel. After stirring for a further two hours at room temperature and for one hour at 50°, the mixture is cooled to 20°, and a solution of 16 g (0.4 mole) of sodium hydroxide in 70 ml of water is added dropwise at 20° in the course of 2 hours. After stirring for a further 2 hours at room temperature and for 6 hours at 60°, a further 16 g (0.4 mole) of sodium hydroxide in 70 ml of water are added dropwise in the course of 2 hours and stirring is continued for a further 5 hours at 60°. After the mixture has cooled to room temperature, 200 ml of water are added, and the precipitate is filtered off after stirring for approx. 30 minutes. The precipitate is thoroughly washed with water, thoroughly suction-drained and dried in vacuo at approx. 95°. The colourless 2,4-bis-allylamino-6-chloro-1,3,5-triazine thus obtained is analytically pure and has a melting point of 205°-206°; its water content is <0.3%. Yield 88.2 g (97.7% of theory).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US04731393 |
|---|
| 出典データセット | uspto-grants-1988_03 |
|---|
| ORD ID | ord-e1b08bff97b54b80b36fe02999720db6 |
|---|
| 出典メモ | uspto-grants-1988_03 |
|---|