2-Amino-5-nitrobenzonitrile → N'-(2-cyano-4-nitrophenyl)-N,N-dimethylmethanimidamide

HRID 240536

반응식

HRID 240536 반응식
[NH2:1][C:2]1[CH:9]=[CH:8][C:7]([N+:10]([O-:12])=[O:11])=[CH:6][C:3]=1[C:4]#[N:5].CO[CH:15](OC)[N:16]([CH3:18])[CH3:17]>>[C:4]([C:3]1[CH:6]=[C:7]([N+:10]([O-:12])=[O:11])[CH:8]=[CH:9][C:2]=1[N:1]=[CH:15][N:16]([CH3:18])[CH3:17])#[N:5]

참가 물질

3

반응물 2

HCID 285322-Amino-5-nitrobenzonitrileHCID 78373Dimethylformamide dimethyl acetal

생성물 1

HCID 10900084N'-(2-cyano-4-nitrophenyl)-N,N-dimethylmethanimidamide수율 87.2%

반응 조건

온도
100 °C

실험 절차

A mixture of 2-amino-5-nitrobenzonitrile (30.0 g, 184 mmol) and dimethoxy-N,N-dimethylmethanamine (29.6 mL, 223 mmol) was heated to 100° C. for 2 hours. The reaction mixture was concentrated under reduced pressure and dissolved in dichloromethane. The solution was run through a silica plug washing the plug with ethyl acetate. The filtrate was concentrated under reduced pressure, stirred with ether and filtered to provide the product (35.0 g, 87%) as yellow solid.

후처리

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. dissolutiondissolved in dichloromethane
  3. washwashing the plug with ethyl acetate
  4. concentrationThe filtrate was concentrated under reduced pressure
  5. filtrationfiltered

출처 및 근거

ORD 기록
ord-5dbd2568eac241eb8ed9e576d7c0f917
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08648087B2

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