3,4-Dimethylaniline → 4-chloro-N-(3,4-dimethyl-phenyl)-3-nitro-benzenesulfonamide

HRID 1514858노트

반응식

HRID 1514858 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([S:8](Cl)(=[O:10])=[O:9])=[CH:4][C:3]=1[N+:12]([O-:14])=[O:13].[CH3:15][C:16]1[CH:17]=[C:18]([CH:20]=[CH:21][C:22]=1[CH3:23])[NH2:19].CN(C1C=CC=CN=1)C>N1C=CC=CC=1>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([NH:19][C:18]2[CH:20]=[CH:21][C:22]([CH3:23])=[C:16]([CH3:15])[CH:17]=2)(=[O:10])=[O:9])=[CH:4][C:3]=1[N+:12]([O-:14])=[O:13]

참가 물질

5

반응물 3

HCID 72483,4-DimethylanilineHCID 7323Benzenesulfonyl chloride, 4-chloro-3-nitro-HCID 218852-Dimethylaminopyridine

생성물 1

HCID 47954984-chloro-N-(3,4-dimethyl-phenyl)-3-nitro-benzenesulfonamide

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

To a solution of 4-chloro-3-nitro-benzenesulfonyl chloride (0.51 g) in pyridine (2 mL) were added 3,4-dimethylaniline and dimethylaminopyridine (0.024 g). The reaction mixture was stirred overnight, concentrated under reduced pressure, and diluted with CH2Cl2. The mixture was washed with water, dried over Na2SO4, and concentrated in vacuo. The residue was purified by column chromatography (SiO2, 1:3 EtOAc/Hexane) to give 4-chloro-N-(3,4-dimethyl-phenyl)-3-nitro-benzenesulfonamide.

후처리

  1. concentrationconcentrated under reduced pressure
  2. additiondiluted with CH2Cl2
  3. washThe mixture was washed with water
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated in vacuo
  6. customThe residue was purified by column chromatography (SiO2, 1:3 EtOAc/Hexane)

출처 및 근거

ORD 기록
ord-b907b49335894d668d476d85cdf71f58
출처 데이터셋
uspto-grants-2012_07
특허 번호
US08222248B2

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