反应详情

A suspension of sodium hydride (2.54 g) in dry dimethylsulphonyl (200 ml) was stirred at room temperature under argon and 1,2,4-triazol 21.9 g) was added in portions over 10 minutes, followed by further stirring for 10 minutes. A solution of 5-bromo-4-(2,4-dichlorophenyl)-4-hydroxy-hex-2-yne (17 g) in dry DMSO (50 ml) was added over 15 minutes. The resultant solution was heated at 100° C. for about 100 hours. Concentrated brine solution (200 ml) was added and the mixture extracted with ethyl acetate (3×150 ml). The extracts were combined, washed with water until neutral, dried over anhydrous magnesium sulphate and the solvent removed in vacuo to give 14.38 g of a brown solid. This solid was purified by flash chromatography, eluted with portions of ethyl acetate (50-100%) in hexane). Fractions containing the fastest running major triazole-active spot on thin-layer chromatography were combined to give 2.91 g (18%) of a white solid.

1. stirringby further stirring for 10 minutes
2. extractionthe mixture extracted with ethyl acetate (3×150 ml)
3. washwashed with water until neutral,
4. dry with materialdried over anhydrous magnesium sulphate
5. customthe solvent removed in vacuo