HRID1165107

反应详情

EQUATION

反应方程式

HRID 1165107 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 25 g (148 mmol) of bromoacetaldehyde dimethyl acetal, 5 mL of water and 5 mL of 48% HBr was refluxed 2 h. After cooling, it was poured into 50 mL of ethanol. Solid sodium bicarbonate was added until bubbling ceased. The mixture was filtered and to the filtrate was added 7.5 g (61 mmol) of 3-amino-4,6-dimethylpyridazine. After stirring 16 h, the ethanol was removed with a rotary evaporator. The residue was triturated with ethanol to give a brown solid which was dissolved in water and washed with dichloromethane. The aqueous layer was brought to pH 9 with sodium bicarbonate and extracted with dichloromethane. Drying (Na2SO4) and solvent removal with a rotary evaporator gave 4 g of the title compound as a brown solid, m.p. 70°-74° C.

WORKUP

后处理

  1. temperaturewas refluxed 2 h
  2. temperatureAfter cooling
  3. customuntil bubbling
  4. filtrationThe mixture was filtered and to the filtrate
  5. customthe ethanol was removed with a rotary evaporator
  6. customThe residue was triturated with ethanol
  7. customto give a brown solid which
  8. washwashed with dichloromethane
  9. extractionextracted with dichloromethane
  10. customDrying
  11. custom(Na2SO4) and solvent removal
  12. customwith a rotary evaporator