Реакция #75559

ord-875dcea2b1ff48fba32f631ed9d15f10

Уравнение реакции

Реагенты

Нет

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ФильтрацияThe mixture was filtered
  2. 2
    Другоеsolvent was evaporated
  3. 3
    workup.ADDITIONEthyl acetate was added
  4. 4
    Другоеinsoluble material was removed by filtration
  5. 5
    ПромывкаThe filtrate was washed with 0.2N HCl, 5% NaHCO3, and saturated aqueous NaCl
  6. 6
    СушкаIt was dried over Na2SO4
  7. 7
    Фильтрацияfiltered
  8. 8
    Другоеevaporate

Методика

Boc-Val-Pro-OBzl was prepared by dissolving H-Pro-OBzl (20 g, 83 mmol) in 50 mL of chloroform and adding Boc-Val-OH (18.0 g, 83 mmol), HOBt (23.0g, 165 mmol), NMM ( 9.0 mL, 83 mmol) and DCC (17.0 g, 83 mmol). The reaction mixture was stirred overnight at room temperature. The mixture was filtered and solvent was evaporated. Ethyl acetate was added and insoluble material was removed by filtration. The filtrate was washed with 0.2N HCl, 5% NaHCO3, and saturated aqueous NaCl. It was dried over Na2SO4, filtered and evaporate to give a white solid (30 g, 75 mmol, 90%). ESI/MS calculated for C22H32N2O5 +H: 405.2. Found 405.6.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US06699855B2uspto-grants-2004_03