Ammonium Chloride → N-(2-iodo-4-nitrophenyl)-N-(methylsulfonyl)methanesulfonamide

HRID 541076

반응식

HRID 541076 반응식
[I:1][C:2]1[CH:8]=[C:7]([N+:9]([O-:11])=[O:10])[CH:6]=[CH:5][C:3]=1[NH2:4].[CH3:12][S:13](Cl)(=[O:15])=[O:14].[NH4+].[Cl-]>ClCCl>[I:1][C:2]1[CH:8]=[C:7]([N+:9]([O-:11])=[O:10])[CH:6]=[CH:5][C:3]=1[N:4]([S:13]([CH3:12])(=[O:15])=[O:14])[S:13]([CH3:12])(=[O:15])=[O:14]

참가 물질

5

반응물 3

HCID 25517Ammonium ChlorideHCID 31297Methanesulfonyl chlorideHCID 2226292-Iodo-4-nitroaniline

생성물 1

HCID 67284344N-(2-iodo-4-nitrophenyl)-N-(methylsulfonyl)methanesulfonamide

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

To a solution of 2-iodo-4-nitroaniline (1.02 g, 3.86 mmol) in dichloromethane (10 ml), has been added under stirring triethylamine (1.77 ml, 12.7 mmol). To this mixture, a solution of methanesulphonyl chloride (0.98 ml, 12.7 mmol) in dichloromethane (2 ml) has been added dropwise, very slowly and in an ice-bath. The mixture so obtained was left under stirring at room temperature overnight. The day after, the reaction mixture was neutralized with a saturated aqueous solution of NH4Cl. The organic phase was separated, and, after evaporation of the solvent, the residue has been washed with ethanol and filtered to give N-(2-iodo-4-nitrophenyl)-N-(methylsulfonyl)-methanesulfonamide as yellow solid.

후처리

  1. customThe mixture so obtained
  2. waitwas left
  3. customThe organic phase was separated
  4. customafter evaporation of the solvent
  5. washthe residue has been washed with ethanol
  6. filtrationfiltered

출처 및 근거

ORD 기록
ord-23c8accabf5148f295a6c4c2ee2b86d0
출처 데이터셋
uspto-grants-2014_10
특허 번호
US08871948B2

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