3-Hydroxy-2-(phenylamino)-4-(phenylimino)-2-cyclobuten-1-one → 1-[2-Hydroxy-3-(cis-3,5-dimethyl-4-ethyl-1-piperazinyl)-4-oxo-2-cyclobuten-1-ylidene]-cis-3,5-dimethyl-4-ethylpiperazinium hydroxide
反応式
[NH:1]([C:8]1[C:9](=[O:20])[C:10](=[N:13][C:14]2[CH:19]=[CH:18]C=CC=2)[C:11]=1[OH:12])[C:2]1[CH:7]=[CH:6]C=CC=1.C[C@H]1CN[CH2:25][C@@H:24]([CH3:28])[N:23]1[CH2:29][CH3:30]>>[OH-:12].[OH:12][C:11]1[C:10](=[N+:13]2[CH2:14][C@H:19]([CH3:18])[N:23]([CH2:29][CH3:30])[C@H:24]([CH3:25])[CH2:28]2)[C:9](=[O:20])[C:8]=1[N:1]1[CH2:2][C@H:7]([CH3:6])[N:1]([CH2:2][CH3:7])[C@H:8]([CH3:9])[CH2:11]1参加物
反応条件
- 温度
- 213 °C
実験手順
A mixture of 1.5 grams of 2-anilino-3-hydroxy-4-(phenylimino)-2-cyclobuten-1-one and 1.2 grams of cis-2,6-dimethyl-1-ethylpiperazine is heated at 213° C. in an atmosphere of dry nitrogen for 10 minutes. It is then mixed thoroughly with 25 ml. of anhydrous ethyl ether and suction filtered and this process is repeated. The solid is then dissolved in 200 ml. of anhydrous ethyl ether at room temperature by stirring for 10 minutes. The solution is then stirred with activated charcoal, filtered, and concentrated to a volume of 25 ml. The solid which forms is separated by filtration to give 1-[2-hydroxy-3-(cis-3,5-dimethyl-4-ethyl-1-piperazinyl)-4-oxo-2-cyclobuten-1-ylidene]-cis-3,5-dimethyl-4-ethylpiperazinium hydroxide inner salt as pale pink crystals melting at about 178°-181° C.
後処理
- additionIt is then mixed thoroughly with 25 ml
- filtrationof anhydrous ethyl ether and suction filtered
- dissolutionThe solid is then dissolved in 200 ml
- stirringThe solution is then stirred with activated charcoal
- filtrationfiltered
- concentrationconcentrated to a volume of 25 ml
- customThe solid which forms is separated by filtration
出典と根拠
- ORDレコード
- ord-d781e271b2db400bb092ddb62bc62a95
- 出典データセット
- uspto-grants-1979_02
- 特許番号
- US04138566
反応ノート
読み込み中…