Реакция #640584

ord-fc313c2da70d4e3490790ff94c8806ae

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Температураcooled
  2. 2
    Экстракцияextracted with ethyl acetate
  3. 3
    ПромывкаThe organic layer was washed with a saturated brine
  4. 4
    Сушкаdried over anhydrous sodium sulfate
  5. 5
    Другоеthe solvent was evaporated under reduced pressure
  6. 6
    ДругоеThe obtained crude crystal
  7. 7
    Промывкаwas washed with a mixture of hexane-ether (2:1)

Методика

2-Nitrobenzyl amine hydrochloride (2.27 g, 12.0 mmol), 3-hydroxy-3-phenyl propionic acid (2.00 g, 12.0 mmol), triethylamine (1.34 g, 13.3 mmol) were added to tetrahydrofuran (50 ml) and the reaction mixture was ice cooled. Under ice cooled condition, 4-(4,6-dimethoxy-1,3,5-triazin-2-yl)-4-methylmorpholinium chloride (3.33 g, 12.0 mmol) was added thereto and stirred at room temperature for five hours. The reaction mixture was poured into dilute hydrochloric acid water and extracted with ethyl acetate. The organic layer was washed with a saturated brine and then dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The obtained crude crystal was washed with a mixture of hexane-ether (2:1) to obtain 3-hydroxy-N-(2-nitrobenzyl)-3-phenyl propionic acid amide (3.32 g).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US08048825B2uspto-grants-2011_11