Tetraethyltin → 2-Ethyl-4,6-dinitroaniline
反応式
[N+:1]([C:4]1[CH:10]=[C:9]([N+:11]([O-:13])=[O:12])[CH:8]=[C:7](Br)[C:5]=1[NH2:6])([O-:3])=[O:2].[CH2:15]([Sn](CC)(CC)CC)[CH3:16]>CN(C=O)C>[N+:1]([C:4]1[CH:10]=[C:9]([N+:11]([O-:13])=[O:12])[CH:8]=[C:7]([CH2:15][CH3:16])[C:5]=1[NH2:6])([O-:3])=[O:2]参加物
4
実験手順
A solution of 2,4-dinitro-6-bromoaniline (1.6 g, 6.1 mmol), tetraethyltin (2.4 ml, 12.2 mmol) and Cl2Pd(PPh3)2 (100 mg) in 10 ml of DMF was stirred at 140° C. for 12 h. Reaction mixture was concentrated in vacuc, yielding an oil which was purified on silica gel column chromatography (CH2Cl2, neat) to provide 0.68 g (3.2 mmol, 33%) of 2,4-dinitro-6-ethylaniline, which was converted to the diamine (0.45 g, 95%) on hydrogenation (H2/Pd—C).
後処理
- customReaction mixture
- concentrationwas concentrated in vacuc
- customyielding an oil which
- customwas purified on silica gel column chromatography (CH2Cl2, neat)
出典と根拠
- ORDレコード
- ord-0b40f1e8e00d4e748d72a58cfa76ccee
- 出典データセット
- uspto-grants-2001_11
- 特許番号
- US06316637B1
反応ノート
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