2-Methyl-5-nitrobenzene-1-sulfonamide → 5-Amino-2-methylbenzenesulfonamide
反応式
[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]参加物
5
実験手順
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+).
後処理
- filtrationThe mixture was filtered through diatomaceous earth
- washthe filter cake was washed with methanol
- concentrationThe combined organic solvents were concentrated under reduced pressure
- customto give crude product, which
- customwas further purified by flash column chromatography (ethyl acetate:hexanes 1:1)
出典と根拠
- ORDレコード
- ord-db99fe3bbabb41c1ad05bb182e7172f2
- 出典データセット
- uspto-grants-2013_07
- 特許番号
- US08497279B2
反応ノート
読み込み中…