Hydrochloric Acid → 3-Amino-5-nitrobenzonitrile
反応式
[N+:1]([C:4]1[CH:5]=[C:6]([CH:9]=[C:10]([N+:12]([O-])=O)[CH:11]=1)[C:7]#[N:8])([O-:3])=[O:2].Cl>CO.[Fe]>[NH2:12][C:10]1[CH:9]=[C:6]([CH:5]=[C:4]([N+:1]([O-:3])=[O:2])[CH:11]=1)[C:7]#[N:8]参加物
5
実験手順
To a suspension of 3,5-dinitrobenzonitrile (4.5 g, 23.30 mmol) in MeOH (100 mL) was added concentrated HCl (15 mL), followed by iron powder (3.90 g, 69.9 mmol). The mixture was stirred at room temperature for 30 min. and then concentrated. The residue was treated with water and the resulting solid product was collected by filtration to give Intermediate 71A (2.3 g, 61%). HPLC: Rt=1.245 min. (CHROMOLITH® column 4.6×50 mm eluting with 10-90% aqueous methanol over 4 min. containing 0.1% TFA, 4 mL/min., monitoring at 220 nm). 1H NMR (500 MHz, DMSO-d6) δ ppm 7.68 (1H, s), 7.64 (1H, s), 7.24 (1H, s), 6.33 (2H, s).
後処理
- concentrationconcentrated
- additionThe residue was treated with water
- filtrationthe resulting solid product was collected by filtration
出典と根拠
- ORDレコード
- ord-9e89093310f64b6a97c8309302f6df43
- 出典データセット
- uspto-grants-2012_08
- 特許番号
- US08252795B2
反応ノート
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