HRID37067

反应详情

EQUATION

反应方程式

HRID 37067 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
37 °C

PROCEDURE

实验过程

2,6-Diaminopurine (Pacific Chemical Laboratories, 0.8 g, 4.8 mmoles) and 1-(2-deoxy-2-fluoro-β-D-ribofuranosyl)uracil (0.4 g, 1.6 mmoles) which may be prepared according to J. F. Codington et al. (J. Org. Chem. 29:558, 1964) were suspended in 50 ml of 5 mM potassium phosphate buffer, pH 7.0, which contained 0.04% (w/w) potassium azide. Thymidine phosphorylase (3,850 I.U.) and purine nucleoside phosphorylase (3,760 I.U.) (T. A. Krenitsky et al., Biochemistry 20:3615, 1981 and U.S. Pat. No. 4,381,344) were added and the suspension stirred at 37° C. On day 12, the reaction was filtered. The filtrate was applied to a 1.5×15 cm column of anion exchange resin (Bio-Rad AG1X2-hydroxide form). After washing the column with water/methanol (7/3), the product was eluted with water/methanol (1/1). Product containing fractions were combined and the solvent removed under vacuum. The residue was dissolved in water and lyophilized to obtain title compound that analyzed as a 1.2 hydrate.

WORKUP

后处理

  1. addition4,381,344) were added
  2. waitOn day 12
  3. filtrationthe reaction was filtered
  4. washAfter washing the column with water/methanol (7/3)
  5. washthe product was eluted with water/methanol (1/1)
  6. additionProduct containing fractions
  7. customthe solvent removed under vacuum
  8. dissolutionThe residue was dissolved in water