반응 #62377

ord-06e895fce5144a5ca92846444e67f562

반응 조건

온도
0°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.STIRRINGstirred at room temperature for 10 minutes
  2. 2
    기타the reaction
  3. 3
    추출After extracting the aqueous phase with ethyl acetate
  4. 4
    세척the organic phase was washed with water and saturated brine
  5. 5
    건조dried over anhydrous magnesium sulfate
  6. 6
    기타The solvent was evaporated

실험 절차

170 mg of furan-2,5-dicarboxylic acid monobenzyl ester was dissolved in 5 mL of tetrahydrofuran, and added with 144 μl of triethylamine. After cooling to 0° C., 72.3 μl of ethyl chloroformate was added dropwise and stirred at this temperature for 30 minutes. 1 mL of concentrated ammonia water was added and stirred at room temperature for 10 minutes, and then aqueous ammonium chloride was added to stop the reaction. After extracting the aqueous phase with ethyl acetate, the organic phase was washed with water and saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated, to afford 185 mg of the title compound as white crystals.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07429609B2uspto-grants-2008_09