HRID485653

反应详情

EQUATION

反应方程式

HRID 485653 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4-(5-Bromo-3-methylpyrid-2-yl)butylamine (0.71 gm) and 2-nitroamino-5-(1-benzyl-2-oxo-pyrid-4-ylmethyl)-4-pyrimidone (1.0 gm) were refluxed in pyridine (3 ml) for 8 hrs., an extra 0.13 gm of the amine was added and reaction was refluxed for a further 5.5 hrs. The pyridine was removed in vacuo, the residue was re-evaporated with n-propanol (2×40 ml). The residue was dissolved in warm ethanol (10 ml) ether added and on cooling a white solid was obtained which was recrystallised from acetonitrile-water (9:1) to give 2-[4-(5-bromo-3-methylpyrid-2-yl)butylamino]-5-(1-benzyl-2-oxo-pyrid-4-ylmethyl)4-pyrimidone (1.18 gm) m.p. 140°-144° C.

WORKUP

后处理

  1. customreaction
  2. temperaturewas refluxed for a further 5.5 hrs
  3. customThe pyridine was removed in vacuo
  4. customthe residue was re-evaporated with n-propanol (2×40 ml)
  5. dissolutionThe residue was dissolved in warm ethanol (10 ml) ether
  6. additionadded
  7. temperatureon cooling a white solid
  8. customwas obtained which
  9. customwas recrystallised from acetonitrile-water (9:1)