HRID1048636

反应详情

EQUATION

反应方程式

HRID 1048636 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of aluminium chloride 6.53 g, sodium azide 9.55 g and tetrahydrofuran 100 mL was stirred with heating under reflux for two hours. The reaction mixtures were cooled under ice-cooling and thereto were added 3-trifluoromethyl-2-methylbenzoic acid chloride and tetrahydrofuran 100 mL and the mixtures were stirred with heating under reflux for ten hours. After cooling the mixtures, to a mixture of sodium nitrite 14.7 g and water 200 mL was added the reaction mixtures with stirring. The mixtures were acidified with concentrated hydrochloric acid and were then extracted with ethyl acetate. The organic layers were dried over anhydrous sodium sulfate and the resulting mixtures were then concentrated under reduced pressure to give 1-(2-methyl-3-trifluoromethylphenyl)-1,4-dihydrotetrazole-5-one.

WORKUP

后处理

  1. temperaturewith heating
  2. temperatureunder reflux for two hours
  3. customThe reaction mixtures
  4. temperaturewere cooled under ice-
  5. temperaturecooling
  6. stirringthe mixtures were stirred
  7. temperaturewith heating
  8. temperatureunder reflux for ten hours
  9. temperatureAfter cooling the mixtures
  10. additionwas added
  11. customthe reaction mixtures
  12. stirringwith stirring
  13. extractionwere then extracted with ethyl acetate
  14. dry with materialThe organic layers were dried over anhydrous sodium sulfate
  15. concentrationthe resulting mixtures were then concentrated under reduced pressure