Реакция #83015

ord-ae228c421e374ea3882f43765a65a3c1

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    workup.STIRRINGThe mixture is stirred for 30 min
  2. 2
    Другоеto reach room temperature
  3. 3
    ПромывкаThe ether layer is successively washed with 5% sodium bicarbonate and brine
  4. 4
    Другоеdried
  5. 5
    workup.STIRRINGstirred at room temperature for 30 min
  6. 6
    ФильтрацияThe precipitate is filtered
  7. 7
    Другоеdried

Методика

A solution of 3,4,4-trifluoro-3-butenoyl chloride (1.97 g, 0.0124 mole) and N-t-Boc-aminoethanol (1.61 g, 0.010 mole) in dry ether (20 mL) is treated with triethylamine (1.25 g, 0.0124 mole) at -78° C. with stirring. The mixture is stirred for 30 min and allowed to reach room temperature and poured in 20 mL of water. The ether layer is successively washed with 5% sodium bicarbonate and brine and dried. The ether solution is saturated with dry HCl gas and stirred at room temperature for 30 min. The precipitate is filtered and dried to give 1.6 g of the title compound as a white solid, a 77% yield. m.p. 94°-100° C.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US05623084uspto-grants-1997_04