Ammonia → HCID 12279048、化合物
反応式
[O:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[C:3]([CH2:10][C:11]#[N:12])=[N:2]1.[Cl-:13].[Al+3].[Cl-].[Cl-].[NH3:17]>Cl>[ClH:13].[O:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[C:3]([CH2:10][C:11]([NH2:17])=[NH:12])=[N:2]1参加物
5
実験手順
A mixture of 1,2-benzisoxazole-3-acetonitrile (0.34 g) and aluminum chloride (0.54 g) was melted at 90° to 100°C, while dry ammonia gas was passed through thereto for 10 minutes. The reaction mixture was dissolved in aqueous ethanolic hydrochloric acid under cooling and then the solvent was distilled off. The residue was dissolved in a small amount of ethanol-chloroform and subjected to silica gel column chromatography and eluted with 10 % methanol-chloroform. The eluates were collected and recrystallized from ethanol to give the desired compound (0.08 g). m.p. 209° to 212°C.
後処理
- customfor 10 minutes
- temperatureunder cooling
- distillationthe solvent was distilled off
- dissolutionThe residue was dissolved in a small amount of ethanol-chloroform
- washeluted with 10 % methanol-chloroform
- customThe eluates were collected
- customrecrystallized from ethanol
出典と根拠
- ORDレコード
- ord-6eb5e01aa90a4bca9041f2a21be36d83
- 出典データセット
- uspto-grants-1976_04
- 特許番号
- US03948928
反応ノート
読み込み中…