反应 #3693607
相关文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:USH0001759
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: A stirred solution of 16.2 grams (0.137 mole) of 1,3-dioxan-4-ylmethanol and 16.7 grams (0.165 mole) of triethylamine in 250 mL of methylene chloride was cooled to about -20° C., and a solution of 17.3 grams (0.151 mole) of methanesulfonyl chloride in about 25 mL of methylene chloride was added dropwise. Upon completion of addition the reaction mixture was allowed to warm to ambient temperature as it stirred for one hour. The reaction mixture was then washed with water and dried with magnesium sulfate. The mixture was filtered and concentrated under reduced pressure to a residue. The residue was purified using column chromatography on silica gel, yielding 18.1 grams of the subject compound. The NMR spectrum was consistent with the proposed structure. Upon completion of addition the reaction mixture The reaction mixture was then washed with water dried with magnesium sulfate The mixture was filtered concentrated under reduced pressure to a residue The residue was purified
来源 ID: ord-18e8703d02b2465b8467d4e10992f5b4