Hydrochloric Acid → 3-Amino-5-nitrobenzonitrile
반응식
[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]참가 물질
5
실험 절차
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).
후처리
- concentrationconcentrated
- additionThe residue was treated with water
- filtrationthe resulting solid product was collected by filtration
출처 및 근거
- ORD 기록
- ord-9e89093310f64b6a97c8309302f6df43
- 출처 데이터셋
- uspto-grants-2012_08
- 특허 번호
- US08252795B2
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