Water → 5-Chloro-2-methyl-3-nitroaniline
反応式
[Cl:1][C:2]1[CH:3]=[C:4]([N+:12]([O-:14])=[O:13])[C:5]([CH3:11])=[C:6]([N+:8]([O-])=O)[CH:7]=1.O.S(S([O-])=O)([O-])=O.[Na+].[Na+]>CO>[Cl:1][C:2]1[CH:3]=[C:4]([N+:12]([O-:14])=[O:13])[C:5]([CH3:11])=[C:6]([NH2:8])[CH:7]=1参加物
5
実験手順
5-Chloro-2-methyl-1,3-dinitro-benzene (1.96 g, from above) was suspended in methanol (80 mL) and water (20 mL) under N2. Sodium dithionite (5.51 g) was added portionwise and the mixture was stirred at room temperature for 3 hr. The reaction mixture was filtered and washed with methanol. The filtrate was then removed under reduced pressure and the residue was partitioned between ethyl acetate (150 mL) and brine (150 mL). The organic layer was dried over magnesium sulfate and evaporated to afford 5-chloro-2-methyl-3-nitro-phenylamine (1.45 g).
後処理
- filtrationThe reaction mixture was filtered
- washwashed with methanol
- customThe filtrate was then removed under reduced pressure
- customthe residue was partitioned between ethyl acetate (150 mL) and brine (150 mL)
- dry with materialThe organic layer was dried over magnesium sulfate
- customevaporated
出典と根拠
- ORDレコード
- ord-0e51da76bfe7483a8f559cf29374efbe
- 出典データセット
- uspto-grants-1999_09
- 特許番号
- US05952362
反応ノート
読み込み中…