반응 #57652

ord-8239c2520776414b9a2e6b0f56193e44

용매

반응 조건

온도
85°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도The mixture was heated
  2. 2
    추출was extracted with ethyl acetate
  3. 3
    추출The organic extract
  4. 4
    세척was washed with water
  5. 5
    건조dried over sodium sulfate
  6. 6
    기타Removal of the solvent in vacuo
  7. 7
    기타gave the crude product, which
  8. 8
    기타was purified by column chromatography

실험 절차

To 3-methyl-4-trifluoromethanesulfonyloxy-benzofuran-2-carboxylic acid tert-butyl ester (190 mg, 0.5 mmol) was added K3PO4 (159 mg, 0.75 mmol), morpholine (52 mg, 0.6 mmol), Pd(OAc)2 (10 mg) and 4 mL of dioxane. The mixture was heated and stirred in an 85° C. oil bath overnight. The reaction mixture was poured into water and was extracted with ethyl acetate. The organic extract was washed with water and dried over sodium sulfate. Removal of the solvent in vacuo gave the crude product, which was purified by column chromatography to give 96 mg of 3-methyl-4-morpholin-4-yl-benzofuran-2-carboxylic acid tert-butyl ester, obtained as white solid.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07420001B2uspto-grants-2008_09