Sodium Dithionite → 4-Methoxy-3-methylsulfanylmethyl-phenylamine
反応式
S(S([O-])=O)([O-])=O.[Na+].[Na+].[CH3:9][O:10][C:11]1[CH:16]=[CH:15][C:14]([N+:17]([O-])=O)=[CH:13][C:12]=1[CH2:20][S:21][CH3:22].C(=O)([O-])O.[Na+]>CO.O>[CH3:9][O:10][C:11]1[CH:16]=[CH:15][C:14]([NH2:17])=[CH:13][C:12]=1[CH2:20][S:21][CH3:22]参加物
5
実験手順
Sodium dithionite (3.264 g) was added to a solution of 1-methoxy-2-methylsulfanylmethyl-4-nitro-benzene (0.8 g), and sodium hydrogen carbonate (1.57 g) in methanol:water (1:1, 200 ml) and stirred at room temperature for 16 h. Solvent was removed at reduced pressure, the residue partitioned between water and ethyl acetate, the organic phase separated, washed with brine dried (Na2SO4) and solvent removed at reduced pressure to give the title compound (0.23 g) as a brown oil. m/z (API+): 184 (MH+).
後処理
- customSolvent was removed at reduced pressure
- customthe residue partitioned between water and ethyl acetate
- customthe organic phase separated
- washwashed with brine
- dry with materialdried (Na2SO4) and solvent
- customremoved at reduced pressure
出典と根拠
- ORDレコード
- ord-7eb1f9319b0a402c825caf499aa87c8f
- 出典データセット
- uspto-grants-2004_03
- 特許番号
- US06699879B1
反応ノート
読み込み中…