Реакция #8442

ord-32bf5b9791c7448ca1a7e797c6eb1088

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ТемператураThe reaction mixture is heated to boiling
  2. 2
    Другоеthe solvent is removed in vac
  3. 3
    ПромывкаThe organic phase is washed with water
  4. 4
    Сушкаdried with magnesium sulfate
  5. 5
    ДругоеAfter removal of the solvent
  6. 6
    Другоеthe residue is chromatographed on silica gel
  7. 7
    Другоеyielding the product

Методика

9.11 g of acetic anhydride, 18.1 g of triethylamine and 0.73 g of dimethylaminopyridine in 400 ml of anhydrous dichloromethane are added to the product from Example A9. The reaction mixture is heated to boiling. When the reaction is complete (monitoring by TLC), the solvent is removed in vac. and the residue is taken up in dichloromethane. The organic phase is washed with water and dried with magnesium sulfate. After removal of the solvent, the residue is chromatographed on silica gel, yielding the product having the following NMR data:

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07087753B2uspto-grants-2006_08