HRID1755872

反应详情

EQUATION

反应方程式

HRID 1755872 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Methylhydrazine (92 mg) (2 mmol) are added at 0° C. to a suspension of 301 mg (1 mmol) of N-[(3,4-dihydro-5-hydroxy-3-methyl-4-oxo-2-pyrimidinyl)methoxy]phthalimide in 9 ml of absolute dimethylformamide. A solution gradually results and this is then stirred at room temperature for 3 hours. The solution is concentrated in a high vacuum at room temperature, the residue is washed with petroleum ether and finally 10 ml of water are added thereto. After good intermixing the mixture is filtered. The filtrate is concentrated, finally with toluene/ethanol. After crystallization from ethanol there are obtained 125 mg of 2-[(aminooxy)methyl]-5-hydroxy-3-methyl-4(3H)-pyrimidinone as white crystals of m.p. 106° C.

WORKUP

后处理

  1. customA solution gradually results
  2. concentrationThe solution is concentrated in a high vacuum at room temperature
  3. washthe residue is washed with petroleum ether and finally 10 ml of water
  4. additionare added
  5. filtrationAfter good intermixing the mixture is filtered
  6. concentrationThe filtrate is concentrated, finally with toluene/ethanol
  7. customAfter crystallization from ethanol