2-Methyl-5-nitrobenzene-1-sulfonamide → 5-Amino-2-methylbenzenesulfonamide

HRID 574195

반응식

HRID 574195 반응식
[NH2:1][S:2]([C:5]1[CH:6]=[C:7]([N+:12]([O-])=O)[CH:8]=[CH:9][C:10]=1[CH3:11])(=[O:4])=[O:3]>ClCCl.CO.[Pd]>[NH2:1][S:2]([C:5]1[CH:6]=[C:7]([CH:8]=[CH:9][C:10]=1[CH3:11])[NH2:12])(=[O:3])=[O:4]

참가 물질

5

반응물 1

HCID 2342822-Methyl-5-nitrobenzene-1-sulfonamide

생성물 1

HCID 2355115-Amino-2-methylbenzenesulfonamide

시약·촉매·용매 3

HCID 23938Palladium촉매HCID 887Methanol용매HCID 6344Dichloromethane용매

실험 절차

To a solution of 3-aminosulfonyl-4-methylnitrobenzene in dichloromethane and methanol was added 10% Pd/C and the mixture shaken under a hydrogen atmosphere at 50 psi for 15 minutes. The mixture was filtered through diatomaceous earth and the filter cake was washed with methanol. The combined organic solvents were concentrated under reduced pressure to give crude product, which was further purified by flash column chromatography (ethyl acetate:hexanes 1:1) to give 3-aminosulfonyl-4-methylaniline, LCMS: purity: 87%; MS (m/e): 187 (MH+).

후처리

  1. filtrationThe mixture was filtered through diatomaceous earth
  2. washthe filter cake was washed with methanol
  3. concentrationThe combined organic solvents were concentrated under reduced pressure
  4. customto give crude product, which
  5. customwas further purified by flash column chromatography (ethyl acetate:hexanes 1:1)

출처 및 근거

ORD 기록
ord-56721924960a473591934342a27241ad
출처 데이터셋
uspto-grants-2015_05
특허 번호
US09034881B2

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