Phosphoric Acid → HCID 70275165, Verbindung

Reaktionsgleichung

P(=O)(O)(O)O.[S:6]1[CH:10]=[CH:9][CH:8]=[C:7]1[CH2:11][CH2:12][N:13]=[C:14]=[S:15].[I:16][CH3:17]>CC(C)=O>[IH:16].[CH3:17][S:15][C:14]1[C:8]2[CH:9]=[CH:10][S:6][C:7]=2[CH2:11][CH2:12][N:13]=1

Komponenten

Versuchsvorschrift

To a stirred solution of phosphoric acid (205 g) at 175° C. was added dropwise 2-(2-thienyl)ethylisothiocyanate (R. V. Davies et al., J. Chem. Soc., Perkin l, 1976, 138). The solution was stirred for 1 h, poured onto ice/water (3 L), the mixture stirred for 3 h to decompose the phosphoric acid, extracted with chloroform, dried over magnesium sulphate and evaporated to give a dark oil which solidified on standing. This solid was taken up in acetone (250 ml) and iodomethane (12 ml) was added. The reaction mixture was stirred for 4 h and the solid was collected to give the title compound as a yellow solid (26 g), m.p. 184-187° C.