반응 #2086

ord-1b88eb8cb6094a9a8d87846b4529cb21

반응 조건

온도
70°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    여과The solution was filtered hot
  2. 2
    기타the dimethylformamide was evaporated under reduced pressure
  3. 3
    세척washed several times with water
  4. 4
    기타After evaporating the solvent, it
  5. 5
    기타without purification

실험 절차

20 g (0.078 mol) of 1-benzyl-3-methylxanthine hydrochloride, 21.4 g (0.094 mol) of diethyl 4-chlorobutanephosphonate and 26 g (0.2 mol) of potassium carbonate were suspended in 400 ml of dimethylformamide and stirred at 70° C. for 6 hours. The solution was filtered hot and the dimethylformamide was evaporated under reduced pressure. The oily residue which remained was taken up in dichloromethane and washed several times with water. After evaporating the solvent, it was possible to reuse the pale yellow, oily residue without purification.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05728686uspto-grants-1998_03