HCID 21874993、化合物 → 5-Amino-3-bromo-2-pyridinecarbonitrile
反応式
[Br:1][C:2]1[C:3]([C:11]#[N:12])=[N:4][CH:5]=[C:6]([N+:8]([O-])=O)[CH:7]=1>[Fe].CCOCC>[NH2:8][C:6]1[CH:7]=[C:2]([Br:1])[C:3]([C:11]#[N:12])=[N:4][CH:5]=1参加物
4
実験手順
3-Bromo-2-cyano-5-nitropyridine (0.4g, 1.75 mmol) and iron powder (0.51g, 8.8 mmol, 325 Mesh) were reacted as described in example 762D. The crude solid obtained by trituration with ether was purified by SiO2 Prep-TLC using 4:1 CH2Cl2/ether as eluent to give compound 769A (0.16 g, (65%) as an off-white solid. HPLC: 100% at 1.77 min(YMC S5 ODS column) eluting with 10–90% aqueous methanol containing 0.2% phosphoric acid over a 4 min gradient monitoring at 220 nm. MS (ES): m/z 197.93 [M+H]+.
後処理
- customwas purified by SiO2 Prep-TLC
出典と根拠
- ORDレコード
- ord-8a62417d22ab4d99b8c219a77f420f03
- 出典データセット
- uspto-grants-2006_11
- 特許番号
- US07141578B2
反応ノート
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