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

HRID 723716Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 723716
[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 (0.4g, 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]+.

Aufarbeitung

  1. customwas purified by SiO2 Prep-TLC

Quellen und Nachweise

ORD-Eintrag
ord-8a62417d22ab4d99b8c219a77f420f03
Quelldatensatz
uspto-grants-2006_11
Patentnummer
US07141578B2

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