反应详情

温度

60 °C

Phenol (6.68 g, 75 mmol) was added to a suspension of sodium hydride (60% dispersion in mineral oil, 2.82 g, 75 mmol) in toluene (50 mL) and the mixture was heated at 60° C. for 2 hours. The temperature was then increased to 80° C. and a solution of 1-(diphenylmethyl)-3-azetidinyl methanesulfonate (15 g, 47 mol) in toluene (150 mL) was added dropwise. The reaction mixture was stirred for 2 hours at 80° C., cooled then washed with water and dilute sodium hydroxide solution. The organic solution was dried over magnesium sulfate, concentrated in vacuo and the residue was re-crystallised from water/isopropanol to afford the title compound as a solid in 84% yield, 12.4 g. LRMS APCI m/z 316 [M+H]+

1. temperatureThe temperature was then increased to 80° C.
2. temperaturecooled
3. washthen washed with water and dilute sodium hydroxide solution
4. dry with materialThe organic solution was dried over magnesium sulfate
5. concentrationconcentrated in vacuo
6. customthe residue was re-crystallised from water/isopropanol