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

HRID 582866

반응식

HRID 582866 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-21a87d10fe224d3e99ec92abe84da1bb
출처 데이터셋
uspto-grants-1999_07
특허 번호
US05925766

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