HRID616251

反应详情

EQUATION

反应方程式

HRID 616251 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of 2-amino-4-chloro-6-hydroxy-5-nitropyrimidine (III) (Hal=Cl) (2.3 g) in dry ethanol was treated with 3-amino-1-hydroxy-3-spirocyclohexylpropan-2-one oxime hydrochloride (IV) (2.5g) and dry triethylamine (2.7 g) and the mixture was refluxed for 7 h. The reaction mixture was filtered and the solid washed with hot ethanol. The solvent was removed from the filtrate and the resulting yellow oil was triturated with cold water giving a yellow solid which on recrystallisation from water in the presence of charcoal gave the nitropyrimidine (II) (1.85 g; yield 47.4%) as an off-white powder, m.pt >300° (decomp.).

WORKUP

后处理

  1. temperaturethe mixture was refluxed for 7 h
  2. filtrationThe reaction mixture was filtered
  3. washthe solid washed with hot ethanol
  4. customThe solvent was removed from the filtrate
  5. customthe resulting yellow oil was triturated with cold water giving a yellow solid which
  6. customon recrystallisation from water in the presence of charcoal