반응 #72192

반응 방정식

methanesulfonyl chloride

Triethylamine

trans(±)-1-(Diphenylmethyl)-2-ethylazetidin-3-ol

→

title compound

수율 90.9%

trans(±)-1-(Diphenylmethyl)-2-ethylazetidin-3-yl methanesulfonate

수율 90.9%

용매

dichloromethane

dichloromethane

ethyl acetate

반응 조건

후처리

1. 1
   세척washed with water and brine
2. 2
   건조dried over anhydrous magnesium sulfate
3. 3
   여과filtration
4. 4
   농축the filtrate was concentrated under reduced pressure
5. 5
   기타The resulting residue was purified by silica gel column chromatography (elution solvent: hexane/ethyl acetate=5/1)

실험 절차

Triethylamine (0.94 mL, 6.74 mmol) was added to a solution of trans(±)-1-(Diphenylmethyl)-2-ethylazetidin-3-ol obtained in Example (234b) (1.20 g, 4.49 mmol) in dichloromethane (8 mL). Then, a solution of methanesulfonyl chloride (0.45 mL, 5.83 mmol) in dichloromethane (1.5 mL) was added dropwise at room temperature, followed by stirring for four hours. The reaction solution was diluted with ethyl acetate, washed with water and brine, and then dried over anhydrous magnesium sulfate. Following filtration, the filtrate was concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography (elution solvent: hexane/ethyl acetate=5/1) to obtain 1.41 g of the title compound as a pale yellow oily substance (91%).

출처