반응 #90144

ord-6bbfad9e6b2844568b529556b7db471e

용매

반응 조건

온도
100°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도under heating
  2. 2
    추출extracted with ethyl acetate
  3. 3
    세척washed with water
  4. 4
    건조The organic layer was dried over magnesium sulfate
  5. 5
    기타The residues obtained
  6. 6
    농축after concentration under reduced pressure
  7. 7
    기타were purified by silica gel column chromatography (ethyl acetate/hexane)

실험 절차

To 2-(1-benzo[b]thiophen-2-yl-1-methylethyl)-4-methoxy-benzoic acid (Compound Z4, 68 mg, 0.22 mmol), polyphosphoric acid (3.5 g) was added, and the mixture was stirred for 1 hr at 100° C. under heating. The mixture was added with water, extracted with ethyl acetate and washed with water. The organic layer was dried over magnesium sulfate. The residues obtained after concentration under reduced pressure were purified by silica gel column chromatography (ethyl acetate/hexane) to obtain the title compound (41 mg, 63%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09440922B2uspto-grants-2016_09