Реакция #62232

ord-87723e92f7c64e559a691aa795a7e25d

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Температураthe reaction mixture was refluxed for 30 min
  2. 2
    ДругоеThe solvent was evaporated under reduced pressure
  3. 3
    Экстракцияthe reaction mixture was extracted with ether (100×3)
  4. 4
    Промывкаthe combined organic phases were washed with water
  5. 5
    Сушкаdried over sodium sulfate and solvent
  6. 6
    Другоеevaporated under reduced pressure
  7. 7
    ДругоеThe crude product was purified by column chromatography (20:80 EA:Hex)

Методика

6.78 g of sodium hydroxide was dissolved in 25 mL of methanol in a 100 mL round bottom flask. The reaction mixture was cooled to room temperature and 60 (6.78 g, 22.90 mmol) was added followed by 5 mL of water and the reaction mixture was refluxed for 30 min. The solvent was evaporated under reduced pressure and the reaction mixture was neutralized with dilute hydrochloric acid and the reaction mixture was extracted with ether (100×3) and the combined organic phases were washed with water and dried over sodium sulfate and solvent evaporated under reduced pressure. The crude product was purified by column chromatography (20:80 EA:Hex) to yield 7.05 g of 61 (quantitative yield).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07429681B2uspto-grants-2008_09