Tripropylamine → HCID 13385683, 화합물

반응식

[F:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[N:8]1[CH:12]=[N:13][N:14]=[C:7]1[C:6](O)=[N:5]2.P(Cl)(Cl)([Cl:18])=O.C(N(CCC)CCC)CC>>[Cl:18][C:6]1[C:7]2[N:8]([CH:12]=[N:13][N:14]=2)[C:9]2[C:4]([N:5]=1)=[CH:3][C:2]([F:1])=[CH:11][CH:10]=2

참가 물질

반응물 3

HCID 7616Tripropylamine

HCID 24813Phosphorus oxychloride

HCID 178517314HCID 178517314, 화합물

생성물 1

HCID 13385683HCID 13385683, 화합물

실험 절차

In a flame-dried reaction flask under a dry nitrogen atmosphere, there were placed 8.9 g. (0.044 mole) of 7-fluoro-4-hydroxy-[1,2,4]triazolo[4,3-a]quinoxaline and 160 ml. of phosphorus oxychloride together with 8.9 ml. of tri-n-propylamine. The reaction mixture was then refluxed overnight for approximately 16 hours and finally cooled to room temperature before being poured over ice/water with mechanical stirring. The resulting aqueous mixture was then stirred at room temperature for 30 minutes and filtered, and the solid product so obtained was subsequently washed with cold water and triturated with ethyl acetate to ultimately afford 7.0 g. (71%) of pure 4-chloro-7-fluoro-[1,2,4]triazolo[4,3-a]quinoxaline, m.p. 305°-308° C. Mass Spectrum: m/e, 222 (P); m/e 224 (P+2).