Water → HCID 21410883, compound

Participants

Reaction Steps

20.3 g (0.1 mol) of β-chloroethyl-phenyl ketone together with 7.6 g (0.1 mol) of thiourea in 100 ml of ethanol in which 0.5% by weight of hydrogen chloride is dissolved, are heated to the boil (for about 3 to 4 hours) until the starting compounds can no longer be detected in a sample by thin-layer chromatography. Thereafter ethanol is azeotropically distilled off whilst toluene is continuously added in the same amount as ethanol distils off and the resulting toluene reaction mixture is boiled for a further 1/2 hour on the water separator. 23 g (about 88% of the theory) of crude 2-amino-4-phenyl-1,3-thiazine hydrochloride (m.p. 204° C.) separate out as faintly yellow-coloured crystals and are filtered off. By recrystallizing from ethanol, pure 2-amino-4-phenyl-1,3-thiazine-hydrochloride is obtained with a melting point of 210° C.

Provenance & Evidence