Water → 2-Methyl-3-nitro-6-(1H-1,2,4-triazol-1-yl)pyridine

HRID 1931572

反応式

HRID 1931572 の反応式
Br[C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[C:4]([CH3:11])[N:3]=1.[NH:12]1[CH:16]=[N:15][CH:14]=[N:13]1.C(=O)([O-])[O-].[K+].[K+].O>CS(C)=O>[CH3:11][C:4]1[C:5]([N+:8]([O-:10])=[O:9])=[CH:6][CH:7]=[C:2]([N:12]2[CH:16]=[N:15][CH:14]=[N:13]2)[N:3]=1

参加物

6

反応物 4

HCID 962WaterHCID 92571H-1,2,4-TriazoleHCID 11430Potassium CarbonateHCID 247280146-Bromo-2-methyl-3-nitropyridine

生成物 1

HCID 579651682-Methyl-3-nitro-6-(1H-1,2,4-triazol-1-yl)pyridine収率 71%

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

実験手順

A mixture of 2-bromo-6-methyl-5-nitropyridine (ECA International Corporation, Palatine, Ill., USA; 2 g, 9.2 mmol), 1,2,4-triazole (Aldrich Chemical Company, Inc., Milwaukee, Wis., USA 0.64 g, 9.2 mmol) and potassium carbonate (1.27 g, 9.2 mmol) in dimethylsulfoxide (4 mL) was stirred at room temperature for 1.5 days and then poured into a mixture of ice and water (400 mL). The resulting mixture was stirred until all of the ice melted to give a dark purple slurry. The solid was filtered off to give 2-methyl-3-nitro-6-[1,2,4]triazol-1-yl-pyridine (1.34 g, 71%) as a purple solid with a purity estimated at 93% by LC-MS. This was used directly in the next step without further purification.

後処理

  1. customto give a dark purple slurry
  2. filtrationThe solid was filtered off

出典と根拠

ORDレコード
ord-be10d49e31754e658bd23079a5bb429e
出典データセット
uspto-grants-2012_05
特許番号
US08188098B2

関連ノート

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