반응 #171268

ord-ccc26b07d9764800a781c225e94306fa

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    추출extracted twice with EtOAc (5 mL)
  2. 2
    세척the combined organic phases were washed with brine (3 mL)
  3. 3
    건조dried with Na2SO4
  4. 4
    농축concentrated

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08846906B2uspto-grants-2014_09