HRID267212

反应详情

EQUATION

反应方程式

HRID 267212 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-Amino-5-methyl-7-propylimidazo[5,1-f]-as-triazine (Example 4) (1.9 g.), p-methoxyacetophenone (1.65 g.) and concentrated hydrochloric acid (2 ml.) in ethanol (50 ml.) were heated under reflux for 1.5 hours. The solvent was distilled off and the residue was treated with 2N sodium carbonate. The mixture was extracted with ethyl acetate and the extract was dried over magnesium sulphate, filtered and evaporated. The residue was crystallised from a mixture of ethyl acetate and light petroleum and had m.p. 193°-195°. The solid in ethanol (20 ml.) was treated with hydrogen chloride in ether. The mixture was further diluted with ether and the solid that crystallised from a mixture of isopropanol and ether and had m.p. 122°.

WORKUP

后处理

  1. temperatureunder reflux for 1.5 hours
  2. distillationThe solvent was distilled off
  3. additionthe residue was treated with 2N sodium carbonate
  4. extractionThe mixture was extracted with ethyl acetate
  5. dry with materialthe extract was dried over magnesium sulphate
  6. filtrationfiltered
  7. customevaporated
  8. customThe residue was crystallised from a mixture of ethyl acetate and light petroleum
  9. additionThe solid in ethanol (20 ml.) was treated with hydrogen chloride in ether
  10. additionThe mixture was further diluted with ether
  11. customthe solid that crystallised from a mixture of isopropanol and ether