반응 #64339

ord-cf15b780d0e5404789b80b8d842efd0d

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타equipped with mechanical stirrer
  2. 2
    온도The mixture was heated for 24 hours
  3. 3
    온도at reflux
  4. 4
    온도cooled
  5. 5
    여과The mixture was filtered
  6. 6
    세척washed with cold methanol (20 ml)

실험 절차

D-Glucurono-6,3-lactone (100.0 g, 0.57 mole), anhydrous methanol (200.0 g, 6.24 moles), and methanesulfonic acid (3 drops) were placed in an oven dried three-necked round bottom flask equipped with mechanical stirrer, thermometer and condenser. The mixture was heated for 24 hours at reflux, cooled and neutralized with 0.1N methanolic KOH. The mixture was filtered and washed with cold methanol (20 ml) yielding 20.9g of methyl β-D-glucofuranosidurono-6, 3-lactone (MβGlucl). By further concentration of the filtrate an additional 28.2 g of MβGlucl was isolated giving a total yield of 49.1 g (45.3%), MP=139, % Purity=99.1.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05412118uspto-grants-1995_05