Water → 4-Methoxy-2-[[(1-methylethylidene)amino]oxy]benzonitrile

HRID 582866

反応式

HRID 582866 の反応式
[CH3:1][C:2](=[N:4][OH:5])[CH3:3].[H-].[Na+].[CH3:8][O:9][C:10]1[CH:17]=[CH:16][C:13]([C:14]#[N:15])=[C:12]([N+]([O-])=O)[CH:11]=1.O>CN(C=O)C>[CH3:8][O:9][C:10]1[CH:17]=[CH:16][C:13]([C:14]#[N:15])=[C:12]([O:5][N:4]=[C:2]([CH3:3])[CH3:1])[CH:11]=1

参加物

6

反応物 4

HCID 962WaterHCID 24758Sodium hydrideHCID 67180Acetone, oximeHCID 2886654-Methoxy-2-nitrobenzonitrile

生成物 1

HCID 187964454-Methoxy-2-[[(1-methylethylidene)amino]oxy]benzonitrile収率 87.2%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

In 20 ml of DMF was dissolved acetone oxime (0.74 g), followed by sodium hydride (0.30 g). After this mixture had stirred for 30 minutes, 4-methoxy-2-nitro-benzonitrile (1.50 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 4-methoxy-2-[[(1-methylethylidene)-amino]oxy]benzonitrile, m.p. 78-79° C.

後処理

  1. filtrationfiltered
  2. customThe solid was collected
  3. dissolutiondissolved in DCM (250 ml)
  4. dry with materialdried (MgSO4)
  5. concentrationconcentrated in vacuo
  6. customThe resulting solid was recrystallized from ethanol

出典と根拠

ORDレコード
ord-21a87d10fe224d3e99ec92abe84da1bb
出典データセット
uspto-grants-1999_07
特許番号
US05925766

関連ノート

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