2-bromo-2-methylpropanoyl bromide

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 2-Bromo-2-methylpropionyl bromide (6.8 mL) was diluted with dichloromethane and added to a solution of triethylamine (7.7 mL) and benzyl alcohol (4.8 mL), while the mixture was cooled in an ice bath and while maintaining an argon atmosphere. The solution was stirred for one hour at 0° C. and then overnight at room temperature. Volatiles were evaporated and the residue was treated with diethylether. The formed salt was removed by filtration and the filtrate was washed with an HCl solution and with water. The ether solution was dried with MgSO4 and concentrated to yield a yellowish liquid. Silica column chromatography using a 2/1 hexane/ethyl acetate mixture as eluent gave a colourless transparent liquid. 1H NMR (400 MHz, CDCl3): δ 7.4 (5H), 5.3 (2H), 2.0 (6H). was cooled in an ice bath while maintaining an argon atmosphere overnight at room temperature Volatiles were evaporated the residue was treated with diethylether The formed salt was removed by filtration the filtrate was washed with an HCl solution and with water The ether solution was dried with MgSO4 concentrated to yield a yellowish liquid gave a colourless transparent liquid