HCID 21874993、化合物 → 5-Amino-3-bromo-2-pyridinecarbonitrile

HRID 2110478ノート

反応式

HRID 2110478 の反応式
[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 (0.4 g, 1.75 mmol) and iron powder (0.51 g, 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

  1. customwas purified by SiO2 Prep-TLC

出典と根拠

ORDレコード
ord-1d4d47d5dcc2446092ad5f0085280875
出典データセット
uspto-grants-2009_04
特許番号
US07517904B2

反応ノート

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