반응 #81561

ord-abf8a50ec94047e1bf23826b5a87330e

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    농축The mixture was concentrated
  2. 2
    추출extracted with ethyl acetate (35 mL×2)
  3. 3
    세척The combined extracts were washed with water (10 mL)
  4. 4
    건조dried over magnesium sulfate
  5. 5
    기타evaporated
  6. 6
    기타The residue was triturated in ether-hexane

실험 절차

Methyl 4-[[(1,1-dimethyl-3-phenyl-1H-inden-5-yl)amino]carbonyl]benzoate (325 mg, 0.82 mmol), 4.1 mL of 2N NaOH in 10 mL of tetrahydrofuran and 10 mL of methanol were stirred for 2 hours. The mixture was concentrated and acidified with 1N HCl (20 mL), extracted with ethyl acetate (35 mL×2). The combined extracts were washed with water (10 mL), dried over magnesium sulfate, and evaporated. The residue was triturated in ether-hexane to give 246 mg (78% yield) of the title compound as white solids; NMR (DMSO-d6) δ1.35 (s, 6H), 6.58 (s, 1H), 7.38-7.70 (m, 7H), 7.73 (d, J=7.9 Hz, 1H), 7.90 (s, 1H), 8.04 (s, 4H), 10.38 (bs, 1H), 13.25 (bs, 1H); MS m/e 384 (MH+).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05618839uspto-grants-1997_04