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380382-24-1

Pyridine, 5-bromo-2-(1H-1,2,4-triazol-1-yl)- synthesis

3synthesis methods
223463-13-6 Synthesis
5-Bromo-2-iodopyridine

223463-13-6
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Pyridine, 5-bromo-2-(1H-1,2,4-triazol-1-yl)-

380382-24-1
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Yield:380382-24-1 1.7 g

Reaction Conditions:

with potassium carbonate in 1-methyl-pyrrolidin-2-one at 100;

Steps:

42 (XX)

(XX)
Scheme XX
Intermediate 441: 5-bromo-2-(1H-1,2,4-triazol-1-yl)pyridine
4.11 g (14.48 mmol) of Compound 440 and 1.2 g (17.38 mmol) of 1,2,4-triazole were dissolved in 10 ml of NMP, added with 4 g (29 mmol) of potassium carbonate, stirred at T=100 °C overnight.
The reaction was reduced to room temperature, and added with 50 ml of ice water to precipitate out solids.
The solid was filtered off, washed with a small amount of ice water, and pumped to dryness to afford a crude product as a white solid (3.257 g).
The crude product was passed through a silica gel chromatographic column to afford a pure product (1.7 g). LC-MS: 225,227 [M+1]+, tR= 1.851 min.

References:

EP3072893,2016,A1 Location in patent:Paragraph 0353; 0354; 0355