反应详情

温度

70 °C

A solution of 12.7 g (0.15 mol) of N-hydroxypyrazole in 20 ml of DMF was added dropwise to a suspension of 4.95 g (1.1 eq.) of NaH (80% dispersion in mineral oil) in 40 ml of DMF at RT, and the mixture was heated at 70° C. for 1 h. A solution of 40.95 g (0.15 mol) of 2-[4-(1,1-dimethylethoxy)phenoxy]ethyl bromide in 100 ml of DMF was added and the mixture was then heated at 125° C. for 15 h. The solvent was then stripped off in a rotary evaporator, the residue was taken up in ethyl acetate, and the solution was washed twice each with 5% strength NaOH solution and water. Drying and removal of the solvent under reduced pressured resulted in 38.4 g (93%) of the required compound as a pale oil which was employed without further purification in the next stage.

1. temperaturethe mixture was then heated at 125° C. for 15 h
2. customThe solvent was then stripped off in a rotary evaporator
3. washthe solution was washed twice each with 5% strength NaOH solution and water
4. customDrying
5. customremoval of the solvent