Methylamine → 2-amino-5-bromopyridine N-methylpyridine-3-carboxamide

HRID 646725ノート

反応式

HRID 646725 の反応式
[NH2:1][C:2]1[C:7]([C:8]([O:10]C)=O)=[CH:6][C:5]([Br:12])=[CH:4][N:3]=1.[CH3:13][NH2:14]>CO>[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([Br:12])=[CH:4][N:3]=1.[CH3:13][NH:14][C:8]([C:7]1[CH:2]=[N:3][CH:4]=[CH:5][CH:6]=1)=[O:10]

参加物

4

反応物 2

HCID 6329MethylamineHCID 2763453Methyl 2-amino-5-bromonicotinate

生成物 1

HCID 686507942-amino-5-bromopyridine N-methylpyridine-3-carboxamide収率 80.6%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
50 °C

実験手順

A slurry of the above methyl 2-amino-5-bromopyridine-3-carboxylate (3.0 g, 13 mmol) in methanol was cooled to 0° C., and methylamine gas was passed through the solution at a moderate rate for 5 min. The mixture was stirred in sealed tube at 50 ° C. for 24 h, and the methanol was removed in vacuo to provide 2-amino-5-bromopyridine-N-methylpyridine-3-carboxamide as a white solid (2.5 g, 80.6% yield): 1H NMR (400 MHz; DMSO-d6): 8.54 (br s, 1H); 8.19 (d, 1H); 8.08 (d, 1H); 7.25 (s, 1H); 2.72 (d, 3H).

後処理

  1. customthe methanol was removed in vacuo

出典と根拠

ORDレコード
ord-8d1c05807d3e454ca61b1d48bae70a08
出典データセット
uspto-grants-2010_04
特許番号
US07704995B2

反応ノート

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