반응 #5104
ord-cebef95bc8384043b4a84d71a6aab475
반응 방정식
반응 조건
후처리
- 1기타had totally formed
- 2기타The reaction mixture was partitioned between water/toluene
- 3기타The organic layer was removed
- 4세척washed with water
- 5기타The organic layer was removed
- 6기타dried
- 7기타evaporated to an orange oil, 5.6 g
- 8기타The oil was chromatographed on 500 g, 90 to 200 mesh silica gel (CH2Cl2 eluent)
실험 절차
To a stirred slurry of 1.6 g sodium hydride (as 50% dispersion in oil) in 50 ml dry dimethyl formamide was added, drop-wise, a solution of 5.0 g p-tert-butylphenol (33.3 mmoles) in 50 ml dry dimethyl formamide and the solution stirred under nitrogen until the phenoxide had totally formed. To the phenoxide was added a solution of 5.0 g 4-chlorobutyl acetate (33.3 mmoles) in 50 ml dry dimethyl formamide and the solution was stirred for fourteen hours. The reaction mixture was partitioned between water/toluene. The organic layer was removed, washed with water, then 1N sodium bicarbonate. The organic layer was removed, dried and evaporated to an orange oil, 5.6 g. The oil was chromatographed on 500 g, 90 to 200 mesh silica gel (CH2Cl2 eluent) yielding pure 4-(p-tert-butylphenoxy)-butyl acetate.