반응 #1095842

ord-4f219fe901ea47398e1918c73013565a

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타to react at 160° C. for 10 minutes
  2. 2
    기타The palladium powder was removed by Kiriyama filtration
  3. 3
    기타the reaction solution was purified by column chromatography (HexH:AcOEt=3:1)

실험 절차

To a DMF solution (0.25 mL) of palladium acetate (38.0 mg, 0.17 μmol), compound 1 (0.50 g, 1.71 mmol), tributylamine (0.41 μL, 1.71 mmol), methyl acrylate (0.38 L, 4.27 mmol), and H2O (1.0 mL) were sequentially added. The reaction solution was allowed to react at 160° C. for 10 minutes using microwaves, and the reaction was traced by TLC. Thereby, the loss of compound 1 was confirmed. The palladium powder was removed by Kiriyama filtration, and then the reaction solution was purified by column chromatography (HexH:AcOEt=3:1), and thus compound 7 (0.26 g, 62%) was obtained as a white powder.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07972792B2uspto-grants-2011_07