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

HRID 1075457노트

반응식

HRID 1075457 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 13387N-methyl-2-pyrrolidone용매

반응 조건

온도
127.5 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d4c1f3c7dba84c46b09e982af156c5dd
출처 데이터셋
uspto-grants-1999_05
특허 번호
US05902813

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