Реакция #171268

ord-ccc26b07d9764800a781c225e94306fa

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Экстракцияextracted twice with EtOAc (5 mL)
  2. 2
    Промывкаthe combined organic phases were washed with brine (3 mL)
  3. 3
    Сушкаdried with Na2SO4
  4. 4
    Концентрированиеconcentrated

Методика

A solution of N-trifluoroacetyl-8-bromo-7-isopropoxy-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine (0.014 g, 0.035 mmol) in methanol (1 mL) was treated with 15% aqueous NaOH (1 mL), and stirred overnight at 20 C. The product mixture was diluted with water (3 mL), extracted twice with EtOAc (5 mL), the combined organic phases were washed with brine (3 mL), dried with Na2SO4 and concentrated to give 0.008 g of a clear oil. 1H NMR (400 MHz, CDCl3) d 7.24 (s, 1H), 6.64 (s, 1H), 4.48 (m, 1H), 2.98 (m, 3H), 2.87 (m, 3H), 1.36 (m, 6H), 1.30 (d, J=7 Hz, 3H). MS calculated for C14H20BrNO+H: 298, observed: 298.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US08846906B2uspto-grants-2014_09