反応 #10965

ord-f8a25e85c5804342b5d24a98cbc5cbf2

反応条件

温度
80°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.ADDITIONafter adding
  2. 2
    その他the solvent was evaporated
  3. 3
    workup.DISTILLATIONby distilling under a reduced pressure
  4. 4
    その他The residue was purified

実験手順

Allyl 3-amino-2-(2-methyl-[1,3]dioxolan-2-yl)propionate (400 mg, 1.86 mmol) was dissolved in 10 mL of chloroform, and 3-fluorophthalic anhydride (401 mg, 2.42 mol) was added to the obtained solution. The resulting mixture was then refluxed at 80° C. for 3 days after adding. After the reaction was completed, the solvent was evaporated by distilling under a reduced pressure. The residue was purified by performing column chromatography (eluent: n-hexane/ethyl acetate=3/1) to obtain the desired product as a white solid (351 mg, 52%). Rf=0.29 (eluent: n-hexane/ethyl acetate=2/1)

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07094908B2uspto-grants-2006_08