Water → 4-Iodo-2-methyl-6-nitroaniline
反応式
[CH3:1][C:2]1[CH:8]=[CH:7][CH:6]=[C:5]([N+:9]([O-:11])=[O:10])[C:3]=1[NH2:4].CC([O-])=O.[Na+].[I:17]Cl.O>C(O)(=O)C>[I:17][C:7]1[CH:6]=[C:5]([N+:9]([O-:11])=[O:10])[C:3]([NH2:4])=[C:2]([CH3:1])[CH:8]=1参加物
6
反応条件
- 温度
- 80 °C
実験手順
To a mixture of 2-methyl-6-nitroaniline (106.5 g, 0.7 mol) and NaOAc (63.2 g, 0.77 mol) in acetic acid (525 mL) was added a solution of ICl (125 g, 0.77 mol) in acetic acid (350 mL). The mixture was heated at 80° C. for 50 min and poured into H2O (2100 mL). After stayed at the room temperature for 16 h, the mixture was filtered to furnish yellow solid that was washed with H2O (3×350 mL). Drying under reduced pressure at 40° C. for 48 h afforded the title compound (191 g, 98%). 1H NMR (CDCl3) δ 2.22 (s, 3H), 6.20 (br s, 2H NH), 7.53 (s, 1H), 8.34 (s, 1H). ESI-MS m/z 279 (MH+).
後処理
- filtrationthe mixture was filtered
- customto furnish yellow solid
- washthat was washed with H2O (3×350 mL)
- customDrying under reduced pressure at 40° C. for 48 h
出典と根拠
- ORDレコード
- ord-7c2f8cecb64f4d928d810c26cf9cf804
- 出典データセット
- uspto-grants-2014_01
- 特許番号
- US08629147B2
反応ノート
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