反应详情

A mixture comprising 1.00 g of methyl N-(5-bromo-2-fluorobenzyl)carbamate, 0.75 g of 3,3-dimethyl-1-butyne, 0.06 g of dichlorobis(triphenylphosphine)palladium, 0.02 g of copper(I) iodide, 1.29 g of triethylamine and 2.7 ml of N,N-dimethylformamide, was stirred at room temperature for 48 hours in a nitrogen atmosphere. This reaction solution was poured into a saturated sodium chloride aqueous solution and extracted with ethyl acetate, followed by drying over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure, and the residue was purified by silica gel column chromatography to obtain 0.40 g of methyl N-[5-(3,3-dimethyl-1-butynyl)-2-fluorobenzyl]carbamate as brown crystals.

1. extractionextracted with ethyl acetate
2. dry with materialby drying over anhydrous magnesium sulfate
3. distillationThe solvent was distilled off under reduced pressure
4. customthe residue was purified by silica gel column chromatography