Thiazole, 2-chloro-4-(trifluoroMethyl)- synthesis

Yield:-

Reaction Conditions:

with tert.-butylnitrite;copper dichloride in acetonitrile at 20; for 3 h;

Steps:

4-(trifluoromethyl)-l,3-thiazol-2-amine (0.25 g, 1.487 mmol), copper(II) chloride (0.240 g, 1.784 mmol), tert-butyl nitrite (0.230 g, 2.230 mmol) were reacted in ACN (20 ml) at room temperature for 3 hours. The reaction mixture was poured into 100 ml 10% aqueous HC1 and extracted with Et₂0 (3x100 ml). The collected organic phases were washed with water, dried over Na₂S0₄, filtered and concentrated at rotavapor at max 650 mBar/35 °C and then in a Claisen apparatus to remove ACN to give the title compound D52 as yellow oil (170 mg).1H NMR (400 MHz, CHLOROFORM-^ δ ppm 7.72 (s, 1 H)

References:

WO2012/89606,2012,A1 Location in patent:Page/Page column 49-50