反应详情

To a suspension of NaH (98 mg, 55% in mineral oil, 2.25 mmol) in DMF (1.2 ml) was added a solution of 4-bromopyrazole (300 mg, 2.04 mmol) in DMF (2 ml). The reaction mixture was stirred at room temperature for 15 minutes before a solution of 3-bromomethyl-3-methyloxetane (404 mg, 2.45 mmol) in DMF (2 ml) was added slowly. The mixture was stirred at room temperature for 1.5 h, then diluted with saturated NaHCO3 solution and extracted with 3 times with EtOAc. The combined organic layers were washed 2 times with water and with brine, dried (Na2SO4) and evaporated. The remaining colorless oil was purified by silica gel chromatography (heptane/EtOAc 80:20-50:50) to obtain the title compound (444 mg, 94%) as colorless oil. MS (EI): 231.2 (M+H)+.

1. additionwas added slowly
2. extractionextracted with 3 times with EtOAc
3. washThe combined organic layers were washed 2 times with water
4. dry with materialwith brine, dried (Na2SO4)
5. customevaporated
6. customThe remaining colorless oil was purified by silica gel chromatography (heptane/EtOAc 80:20-50:50)