Sodium Hydroxide → 7-Chloro-[1,2,4]triazolo[1,5-a]pyrimidine

反応式

[N:1]1[N:5]2[C:6](O)=[CH:7][CH:8]=[N:9][C:4]2=[N:3][CH:2]=1.P(Cl)(Cl)([Cl:13])=O.[OH-].[Na+]>>[Cl:13][C:6]1[N:5]2[N:1]=[CH:2][N:3]=[C:4]2[N:9]=[CH:8][CH:7]=1

参加物

反応物 3

HCID 14798Sodium Hydroxide

HCID 24813Phosphorus oxychloride

HCID 178516466HCID 178516466、化合物

生成物 1

HCID 217666127-Chloro-[1,2,4]triazolo[1,5-a]pyrimidine

実験手順

5.4 g of [1,2,4]triazolo[1,5-a]pyrimidin-7-ol from the first synthesis step are introduced into 20 ml of phosphorus oxychloride with vigorous stirring. After completion, the mixture is warmed under reflux for a further 1.5 h. For work-up, the cooled batch is stirred in portions into 100 ml of ice-water and subsequently adjusted to pH 12 using conc. NaOH solution. The aqueous phase is extracted with ethyl acetate. The combined organic phases are dried over sodium sulfate, and the solvent is removed in vacuo. The 7-chloro-[1,2,4]triazolo[1,5-a]pyrimidine obtained is employed in the following reaction without further purification; m.p. 190° [lit. 186-187° C.];