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

HRID 2378460Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2378460
[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-7bf6e365ff0649418772ef9ec66e25a9
Quelldatensatz
uspto-grants-2008_12
Patentnummer
US07470797B2

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