Dimethylamine → (E)-3-(2-(Dimethylamino)vinyl)-4-nitropyridine 1-oxide

HRID 2201790노트

반응식

HRID 2201790 반응식
[CH3:1][C:2]1[CH:3]=[N+:4]([O-:11])[CH:5]=[CH:6][C:7]=1[N+:8]([O-:10])=[O:9].CNC.O.[CH3:16][N:17]([CH3:20])[CH:18]=O>>[CH3:16][N:17]([CH3:20])/[CH:18]=[CH:1]/[C:2]1[CH:3]=[N+:4]([O-:11])[CH:5]=[CH:6][C:7]=1[N+:8]([O-:10])=[O:9]

참가 물질

5

반응물 4

HCID 674DimethylamineHCID 962WaterHCID 6228Dimethylformamide2회HCID 70633Pyridine, 3-methyl-4-nitro-, 1-oxide

생성물 1

HCID 11344817(E)-3-(2-(Dimethylamino)vinyl)-4-nitropyridine 1-oxide수율 50%

반응 조건

온도
90 °C

실험 절차

To the stirred solution of 3-methyl-4-nitropyridine 1-oxide (600 mg, 3.8 mmol, Step b) in dimethylformamide was added dimethylformamide and dimethylamine (1.14 mL, 8.5 mmol) drop wise at room temperature. After complete addition, the reaction mixture was stirred at 90° C. for 15 hours. The reaction mixture was poured on cold water and the precipitated solid was filtered, washed with water and dried to get (E)-N,N-dimethyl-2-(4-nitro-1-oxidopyridin-3-yl)ethenamine (470 mg, 50%).

후처리

  1. additionAfter complete addition
  2. filtrationthe precipitated solid was filtered
  3. washwashed with water
  4. customdried

출처 및 근거

ORD 기록
ord-d434a110303245b1b55d884c5c5a04e5
출처 데이터셋
uspto-grants-2016_06
특허 번호
US09364466B2

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