関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 1,3,5-Triazin-2-amine, N,4-dicyclopropyl-6-(4-morpholinyl)-, monohydrochloride | HCID 3073348 | — |
| 反応物 | Diethyl ether ethanol | HCID 21585056 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 2-Cyclopropyl-4-cyclopropylamino-6-morpholino-1,3,5-triazine | HCID 3073349 | — |
反応手順
2.85 g (0.050 mole) of cyclopropylamine dissolved in 20 ml of dioxane are added to a solution of 5.1 g (0.021 mole) of 2-chloro-4-cyclopropyl-6-morpholino-1,3,5-triazine in 50 ml of dioxane at room temperature. The mixture is heated under reflux for 5 hours. The solvent is then evaporated under reduced pressure and the residue is dissolved in 50 ml of dichloromethane and 50 ml of water. The organic phase is separated off and dried over sodium sulfate and the solvent is evaporated under reduced pressure. The residue crystallizes from cold hexane. 5.22 g of product are obtained. This product forms a hydrochloride in an ethanol-diethyl ether mixture. 5.1 g of 2-cyclopropyl-4-cyclopropylamino-6-morpholino-1,3,5-triazine hydrochloride, which is identical to compound 3 prepared in example 2. B.1., are obtained. Yield: 81.7%. M.P.: 183°-184° C. (acetonitrile).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05258513 |
|---|
| 出典データセット | uspto-grants-1993_11 |
|---|
| ORD ID | ord-1d0d5a106dfd4eb3ad90504e0a42a37f |
|---|
| 出典メモ | uspto-grants-1993_11 |
|---|