Sodium sulfide nonahydrate → 5-Fluoro-2-methyl-3-nitroaniline
反応式
[N+:1]([C:4]1[CH:9]=[C:8]([F:10])[CH:7]=[C:6]([N+:11]([O-])=O)[C:5]=1[CH3:14])([O-:3])=[O:2].O.O.O.O.O.O.O.O.O.[S-2].[Na+].[Na+]>C(O)C.O>[NH2:11][C:6]1[CH:7]=[C:8]([F:10])[CH:9]=[C:4]([N+:1]([O-:3])=[O:2])[C:5]=1[CH3:14]参加物
5
実験手順
A solution of 2,6-dinitro-4-fluorotoluene (8.1 g) in ethanol (130 mL) is treated dropwise with a solution of sodium sulfide nonahydrate (16.39 g) in water (90 mL). The mixture is allowed to stir at room temperature for 2.5 hours, then diluted with water (500 mL) and extracted with ethyl acetate (4×500 mL). The combined extracts are dried over sodium sulfate and rotary evaporated. The residue is purified by flash chromatography on silica gel, eluting with 15% ethyl acetate/hexanes to afford 2-amino-4-fluoro-6-nitrotoluene as a solid.
後処理
- extractionextracted with ethyl acetate (4×500 mL)
- dry with materialThe combined extracts are dried over sodium sulfate and rotary evaporated
- customThe residue is purified by flash chromatography on silica gel
- washeluting with 15% ethyl acetate/hexanes
出典と根拠
- ORDレコード
- ord-8d1699e30dd6444e941f08c279f513ec
- 出典データセット
- uspto-grants-1999_06
- 特許番号
- US05916900
反応ノート
読み込み中…