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

HRID 1441856Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1441856
[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-fcd2257e991e497b96f66790d3d8a7e5
Quelldatensatz
uspto-grants-2010_02
Patentnummer
US07655689B2

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