Triethylamine → trans(+/-)-1-(Diphenylmethyl)-2-ethylazetidin-3-yl methanesulfonate

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%).

1. washwashed with water and brine
2. dry with materialdried over anhydrous magnesium sulfate
3. filtrationfiltration
4. concentrationthe filtrate was concentrated under reduced pressure
5. customThe resulting residue was purified by silica gel column chromatography (elution solvent: hexane/ethyl acetate=5/1)

ORD-Eintrag

ord-cc578f873d52450a8f3a9610a5a267d0

Quelldatensatz

uspto-grants-2015_01

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08927588B2