반응 #2148

ord-5fefdaf5b899469aa937eb0977a556aa

반응 방정식

[H-].[Na+]
sodium hydride
O=c1[nH]c(=O)n(-c2ccccc2)c2nc[nH]c12
3-phenylxanthine
BrCc1ccccc1
benzyl bromide
O=c1[nH]c(=O)n(-c2ccccc2)c2ncn(Cc3ccccc3)c12
7-Benzyl-3-phenylxanthine

용매

반응 조건

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

후처리

  1. 1
    온도heated to 80° C
  2. 2
    workup.WAITthe solution was left at 80° C. for 6 hours
  3. 3
    온도After cooling to 50° C.
  4. 4
    기타the precipitate obtained
  5. 5
    여과was filtered off with suction
  6. 6
    세척washed well with water
  7. 7
    기타dried under reduced pressure
  8. 8
    기타The dry residue was crystallized from dioxane/methanol

실험 절차

3.2 g (0.1315 mol) of sodium hydride were added in portions to a suspension of 30 g (0.1315 mol) of 3-phenylxanthine in 600 ml of DMF, the mixture was stirred at 25° C. for 30 minutes and then heated to 80° C. 27 g (0.1578 mol) of benzyl bromide were then added and the solution was left at 80° C. for 6 hours. After cooling to 50° C., the reaction mixture was poured into 2000 ml of ice-water, and the precipitate obtained was filtered off with suction, washed well with water and dried under reduced pressure. The dry residue was crystallized from dioxane/methanol.

출처

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