反应 #62377

ord-06e895fce5144a5ca92846444e67f562

反应条件

温度
0°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.STIRRINGstirred at room temperature for 10 minutes
  2. 2
    其他the reaction
  3. 3
    萃取After extracting the aqueous phase with ethyl acetate
  4. 4
    洗涤the organic phase was washed with water and saturated brine
  5. 5
    干燥dried over anhydrous magnesium sulfate
  6. 6
    其他The solvent was evaporated

实验过程

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.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07429609B2uspto-grants-2008_09