반응 #6348

ord-bcb1f28502a14261b19c5dc4802361c3

반응 조건

온도
25°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    여과The suspension was then filtered
  2. 2
    세척the catalyst washed with ethanol
  3. 3
    기타The filtrate was evaporated under reduced pressure
  4. 4
    기타the resulting solid triturated with ether
  5. 5
    기타The solid was collected
  6. 6
    기타dried

실험 절차

A mixture of 9-benzyloxy-6-phthalimidopurine (11.0 g, 29.5 mmol), 10% palladium on charcoal (2.2 g), ethanol (300 ml) and tetrahydrofuran (500 ml) was stirred at 25° C. for 1 hour under an atmosphere of hydrogen. The suspension was then filtered and the catalyst washed with ethanol. The filtrate was evaporated under reduced pressure and the resulting solid triturated with ether. The solid was collected and then dried to afford the title compound (6.93 g; 83%). IR: νmax (KBr). 2607, 1794, 1735, 1603, 1582, 1467, 1401 cm-1 ; 1H NMR δH [(CD3)2SO] 8.15(4H, s, Ar), 8.95(1H, s, H-2), 9.15(1H, s, H-8), 12.80(1H, br.s, D2O exchangeable, OH). Found: C, 55.34; H, 2.58; N, 24.56%. C13H7N5O3 requires: C, 55.51; H, 2.51; N, 24.91%.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05247085uspto-grants-1993_09