Реакция #62391

ord-386231fe66e54a26bac7d782698e1a68

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ЭкстракцияAdding water, extracting with chloroform
  2. 2
    Промывкаthe resultant organic layer was washed with saturated brine
  3. 3
    Сушкаdried over magnesium sulfate
  4. 4
    ДругоеThe solvent was evaporated
  5. 5
    Другоеfollowed by purification by silica gel column chromatography (ethyl acetate:hexane=1:4)

Методика

13.5 g of N-methyl-hydrazine carboxylic acid tert-butyl ester was dissolved in 90 mL of chloroform, added with 90 mL of 1N sodium hydroxide aqueous solution and 28 mL of benzyl chloroformate, and stirred at room temperature for 6 days. Adding water, extracting with chloroform, and the resultant organic layer was washed with saturated brine and dried over magnesium sulfate. The solvent was evaporated, followed by purification by silica gel column chromatography (ethyl acetate:hexane=1:4), to afford 17.7 g of the title compound as a colorless oil.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07429609B2uspto-grants-2008_09