反応 #3733

ord-fe8f501adbbe4ac2972456200d435247

反応方程式

CCCCn1c(=O)c2[nH]c(Br)nc2n(CCCC)c1=O
1,3-Di-n-butyl-8-bromo xanthine
C1CCNCC1
piperidine
CCCCn1c(=O)c2[nH]c(N3CCCCC3)nc2n(CCCC)c1=O
title product
CCCCn1c(=O)c2[nH]c(N3CCCCC3)nc2n(CCCC)c1=O
1,3-Di-n-butyl-8-piperidino Xanthine

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度was refluxed for 9 hours
  2. 2
    抽出The reaction mixture was then extracted with water (4×30 ml)
  3. 3
    乾燥the organic layer dried over anhydrous sodium sulphate
  4. 4
    その他the solvent removed in vacuo
  5. 5
    その他The residue was recrystallised from ethanol

実験手順

1,3-Di-n-butyl-8-bromo xanthine (2 g, 0.0029 mol) was dissolved in toluene (50 ml). After addition of piperidine (5 g, 0.0058 mol) the mixture was refluxed for 9 hours. The reaction mixture was then extracted with water (4×30 ml), the organic layer dried over anhydrous sodium sulphate and the solvent removed in vacuo. The residue was recrystallised from ethanol to give the title product, yield 0.4 g (20%), m.pt. 221° C.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05734051uspto-grants-1998_03