Реакция #64339

ord-cf15b780d0e5404789b80b8d842efd0d

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Другоеequipped with mechanical stirrer
  2. 2
    ТемператураThe mixture was heated for 24 hours
  3. 3
    Температураat reflux
  4. 4
    Температураcooled
  5. 5
    ФильтрацияThe mixture was filtered
  6. 6
    Промывкаwashed with cold methanol (20 ml)

Методика

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.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US05412118uspto-grants-1995_05