Water → 4-Chloro-2-[[(1-methylethylidene)amino]oxy]benzonitrile
反応式
[CH3:1][C:2](=[N:4][OH:5])[CH3:3].CC(C)([O-])C.[K+].[Cl:12][C:13]1[CH:20]=[CH:19][C:16]([C:17]#[N:18])=[C:15]([N+]([O-])=O)[CH:14]=1.O>CN(C)C=O>[Cl:12][C:13]1[CH:20]=[CH:19][C:16]([C:17]#[N:18])=[C:15]([O:5][N:4]=[C:2]([CH3:3])[CH3:1])[CH:14]=1参加物
6
実験手順
In 75 ml of dry N,N-dimethylformamide was dissolved acetone oxime (1.21 g), followed by potassium tertiary butoxide (1.85 g) and stirred under nitrogen. After 30 minutes, 4-chloro-2-nitro-benzonitrile (2.00 g) was added. After an additional 30 minutes the reaction was poured into water (500 ml) and filtered. The solid was collected and dissolved in DCM (250 ml), dried (MgSO4), and concentrated in vacuo. The resulting solid was recrystallized from ethanol to yield 1.5 g of the product, m.p. 83-84° C.
後処理
- filtrationfiltered
- customThe solid was collected
- dissolutiondissolved in DCM (250 ml)
- dry with materialdried (MgSO4)
- concentrationconcentrated in vacuo
- customThe resulting solid was recrystallized from ethanol
出典と根拠
- ORDレコード
- ord-b0496799b6cd46ba84d9201c0b9b6e22
- 出典データセット
- uspto-grants-1999_07
- 特許番号
- US05925766
反応ノート
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