반응 #46336

ord-08c2fc198f4548609bed8b6b0ac4c2b7

반응 조건

온도
20°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The mixture obtained
  2. 2
    기타is separated
  3. 3
    건조the organic phase is dried over magnesium sulfate
  4. 4
    여과filtered
  5. 5
    농축concentrated to dryness under reduced pressure (2.7 kPa)

실험 절차

1-(3-Methylsulfonylmethylphenyl)azetidine may be prepared by carrying out the procedure in the following manner: a solution of 1.9 g of 1-(3-methylsulfanylmethylphenyl)azetidine in 10 cm3 of ethanol is added to a mixture, cooled to 0° C., of 10 cm3 of water, 5 cm3 of acetic acid, 1.5 cm3 of 36 N sulfuric acid and 6.15 g of oxone. After stirring for 20 hours at 20° C., the reaction mixture is supplemented with 100 cm3 of water, 100 cm3 of ethyl acetate and is then neutralized by stirring with sodium hydrogen carbonate. The mixture obtained is separated after settling, the organic phase is dried over magnesium sulfate and then filtered and concentrated to dryness under reduced pressure (2.7 kPa). 1.55 g of 1-(3-methylsulfonyl-methylphenyl)azetidine are obtained in the form of a light brown gum.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07741316B2uspto-grants-2010_06