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

HRID 1441856ノート

反応式

HRID 1441856 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

反応物 1

HCID 21874993HCID 21874993、化合物

生成物 1

HCID 218752405-Amino-3-bromo-2-pyridinecarbonitrile

試薬・触媒・溶媒 2

HCID 23925Iron触媒HCID 3283Diethyl Ether溶媒

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-fcd2257e991e497b96f66790d3d8a7e5
出典データセット
uspto-grants-2010_02
特許番号
US07655689B2

反応ノート

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