Potassium Carbonate → 2-[3-[(E)-2-(5-bromopyridin-3-yl)vinyl]phenylamino]-3-nitropyridine

HRID 1953406ノート

反応式

HRID 1953406 の反応式
[NH2:1][C:2]1[CH:3]=[C:4](/[CH:8]=[CH:9]/[C:10]2[CH:11]=[N:12][CH:13]=[C:14]([Br:16])[CH:15]=2)[CH:5]=[CH:6][CH:7]=1.Cl[C:18]1[C:23]([N+:24]([O-:26])=[O:25])=[CH:22][CH:21]=[CH:20][N:19]=1.C(=O)([O-])[O-].[K+].[K+]>O1CCOCC1>[Br:16][C:14]1[CH:15]=[C:10](/[CH:9]=[CH:8]/[C:4]2[CH:3]=[C:2]([NH:1][C:18]3[C:23]([N+:24]([O-:26])=[O:25])=[CH:22][CH:21]=[CH:20][N:19]=3)[CH:7]=[CH:6][CH:5]=2)[CH:11]=[N:12][CH:13]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 796132-Chloro-3-nitropyridineHCID 232980903-[(E)-2-(3-aminophenyl)vinyl]-5-bromopyridine

生成物 1

HCID 232980802-[3-[(E)-2-(5-bromopyridin-3-yl)vinyl]phenylamino]-3-nitropyridine収率 32.3%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

A mixture of 3-[(E)-2-(3-aminophenyl)vinyl]-5-bromopyridine (3.5 g), 2-chloro-3-nitropyridine (2.22 g) and potassium carbonate (2.64 g) in 1,4-dioxane (30 ml) was stirred under reflux for 22 hours. The mixture was filtered and the filtrate was concentrated. The resultant solid was washed with ethanol to give 2-[3-[(E)-2-(5-bromo pyridin-3-yl)vinyl]phenylamino]-3-nitropyridine (1.63 g).

後処理

  1. temperatureunder reflux for 22 hours
  2. filtrationThe mixture was filtered
  3. concentrationthe filtrate was concentrated
  4. washThe resultant solid was washed with ethanol

出典と根拠

ORDレコード
ord-3bbdde44f9b74d4c8d5e339989e2de7e
出典データセット
uspto-grants-2000_09
特許番号
US06117875

反応ノート

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