반응 #57634

ord-e097fe578d814ac1a945e082a61e03c5

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
    여과Filtration
  7. 7
    기타followed by removal of the solvent in vacuo
  8. 8
    기타gave the crude product (71 mg), which
  9. 9
    기타was purified by column chromatography

실험 절차

3-Methyl-4-trifluoromethanesulfonyloxy-benzofuran-2-carboxylic acid tert-butyl ester (85 mg, 0.25 mmol) was mixed with K2CO3 (68 mg, 0.5 mmol), phenylboronic acid (31 mg, 0.25 mmol), Pd(Ph3)4 (14 mg, 0.01 mmol), 1 mL of 1,2-dimethoxyethane and 2 drops of water. The mixture was heated and stirred in an 85° C. oil bath for 2 h. 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. Filtration followed by removal of the solvent in vacuo gave the crude product (71 mg), which was purified by column chromatography to give 53 mg (77% yield) of 3-methyl-4-phenyl-benzofuran-2-carboxylic acid tert-butyl ester, obtained as white solid.

출처

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