HCID 21874993, Verbindung → 5-Amino-3-bromo-2-pyridinecarbonitrile

HRID 2110478Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2110478
[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

Komponenten

4

Versuchsvorschrift

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]+.

Aufarbeitung

  1. customwas purified by SiO2 Prep-TLC

Quellen und Nachweise

ORD-Eintrag
ord-1d4d47d5dcc2446092ad5f0085280875
Quelldatensatz
uspto-grants-2009_04
Patentnummer
US07517904B2

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