Water → N-(3-(3-Pyridyl)phenyl)-2-nitro-4-(1-pyrrolyl)aniline

HRID 1075457ノート

反応式

HRID 1075457 の反応式
[N+:1]([C:4]1[CH:9]=[C:8]([N:10]2[CH:14]=[CH:13][CH:12]=[CH:11]2)[CH:7]=[CH:6][C:5]=1F)([O-:3])=[O:2].[N:16]1[CH:21]=[CH:20][CH:19]=[C:18]([C:22]2[CH:23]=[C:24]([CH:26]=[CH:27][CH:28]=2)[NH2:25])[CH:17]=1.O.[OH-].[Na+]>CN1CCCC1=O>[N:16]1[CH:21]=[CH:20][CH:19]=[C:18]([C:22]2[CH:23]=[C:24]([NH:25][C:5]3[CH:6]=[CH:7][C:8]([N:10]4[CH:14]=[CH:13][CH:12]=[CH:11]4)=[CH:9][C:4]=3[N+:1]([O-:3])=[O:2])[CH:26]=[CH:27][CH:28]=2)[CH:17]=1

参加物

6

反応物 4

HCID 962WaterHCID 14798Sodium HydroxideHCID 4595213-(Pyridin-3-yl)anilineHCID 541021862-Nitro-4-(1-pyrrolyl)fluorobenzene

生成物 1

HCID 54302123N-(3-(3-Pyridyl)phenyl)-2-nitro-4-(1-pyrrolyl)aniline

試薬・触媒・溶媒 1

HCID 13387N-methyl-2-pyrrolidone溶媒

反応条件

温度
127.5 °C

実験手順

A mixture of 1a (0.5g, 2.4mmol) and 2a (0.41g, 2.4mmol) in N-methyl-2-pyrrolidone (2.5ml) is heated to 120-135° C. for 2 days. After cooling water and diluted sodium hydroxide is added and the mixture is extracted with ethyl acetate. The extract is dried over sodium sulfate, and the solvent is evaporated to leave crude 3a. This crude product is purified by column-chromatography on silica gel using dichloromethane and subsequently a mixture of dichloromethane and methanol (9:1) as the eluents to yield pure 3a (0.61g, 71%) as an oil.

後処理

  1. additionis added
  2. extractionthe mixture is extracted with ethyl acetate
  3. dry with materialThe extract is dried over sodium sulfate
  4. customthe solvent is evaporated

出典と根拠

ORDレコード
ord-d4c1f3c7dba84c46b09e982af156c5dd
出典データセット
uspto-grants-1999_05
特許番号
US05902813

反応ノート

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