Water → HCID 11749519, compound

Participants

Reaction Conditions

Reaction Steps

n-Butyl lithium (6.04 mL, 2.5 mmol) was slowly added over a 15 min period to 3-(2-chloro-6-fluorophenyl)-5-(3-methyl-4,5-dibromothien-2-yl) 1-methyl [1,2,4] triazole (7.0 g) in THF (100 mL) at −70° C. under a nitrogen atmosphere and stirred for 1.0 h. After the addition of the distilled water, the reaction was allowed to warm to 25° C. The reaction mixture was extracted with diethyl ether (3×100 mL). The combined ether extracts was washed with water, dried over anhydrous sodium sulfate, filtered and concentrated to crude solid. This was chromatographed on silica gel (EtOAc/Hexane, 1:1) to give 5.0 g (86% yield) 3-(2-chloro-6-fluorophenyl)-5-(3-methyl-4-bromothien-2-yl) 1-methyl [1,2,4] triazole as white solid. MP 111-112° C. ; Anal. Calcd. For C14H10BrClFN3S: C, 43.49; H, 2.61; N, 10.87; S, 8.29. Found; C, 43.79; H, 2.66; N, 10.95; S, 8.28.

Provenance & Evidence