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

HRID 2201790ノート

反応式

HRID 2201790 の反応式
[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]

参加物

5

反応物 4

HCID 674DimethylamineHCID 962WaterHCID 6228Dimethylformamide2 回HCID 70633Pyridine, 3-methyl-4-nitro-, 1-oxide

生成物 1

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

反応条件

温度
90 °C

実験手順

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%).

後処理

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

出典と根拠

ORDレコード
ord-d434a110303245b1b55d884c5c5a04e5
出典データセット
uspto-grants-2016_06
特許番号
US09364466B2

反応ノート

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