反応式
[N:1]1([CH2:6][C:7]([C:9]2[CH:14]=[CH:13][C:12]([Cl:15])=[CH:11][CH:10]=2)=[O:8])[CH:5]=[N:4][CH:3]=[N:2]1.[BH4-].[Na+]>CO>[Cl:15][C:12]1[CH:13]=[CH:14][C:9]([CH:7]([OH:8])[CH2:6][N:1]2[CH:5]=[N:4][CH:3]=[N:2]2)=[CH:10][CH:11]=1参加物
4
実験手順
A suspension of α-1,2,4-triazol-1-yl-p-chloroacetophenone (4 g) in methanol (12 ml) was treated with sodium borohydride (0.5 g) with cooling and stirring. The mixture was then left at room temperature for 0.5 hour and refluxed for 1 hour. The methanol was removed under reduced pressure and water (25 ml) was added followed by dilute hydrochloric acid (10 ml). The white solid was filtered, washed with water and dried. Crystallisation from ethyl acetate-petroleum ether (60°-80°) gave the title compound as a white crystalline solid. Analysis:
後処理
- temperaturewith cooling
- temperaturerefluxed for 1 hour
- customThe methanol was removed under reduced pressure and water (25 ml)
- additionwas added
- filtrationThe white solid was filtered
- washwashed with water
- customdried
- customCrystallisation from ethyl acetate-petroleum ether (60°-80°)
出典と根拠
- ORDレコード
- ord-aec6030bdd3e4464948156ea7dbc710f
- 出典データセット
- uspto-grants-1983_07
- 特許番号
- US04394380
関連ノート
読み込み中…