[BH4-].[Na+].[NH2:3][C:4]1[CH:9]=[CH:8][CH:7]=[C:6]([Cl:10])[C:5]=1[C:11](=O)[CH3:12].[C:14]([S-:16])#[N:15].[K+].Cl>C(O)C.CCCCCCC.C(OCC)(=O)C.O>[Cl:10][C:6]1[CH:7]=[CH:8][CH:9]=[C:4]2[C:5]=1[CH:11]([CH3:12])[NH:15][C:14](=[S:16])[NH:3]2At a temperature of 65° C., sodium borohydride was added to a solution of 1-(2-amino-6-chloro-phenyl)-ethanone in ethanol, and the mixture was heated overnight (65° C.). Water, KSCN and HCl were then added subsequently, and the mixture was again heated (3 h, 65° C.). The majority of the title compound precipitated upon cooling and could be isolated in sufficiently pure form by filtration. A small additional amount of the desired product was obtained by workup of the mother liquor (evaporation of solvent, column chromatography [silica gel, solvent gradient n-heptan/ethyl acetate=100/0−60/40]). The title compound was obtained in a combined yield of 1.46 g (43%).
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