HRID1048617

反应详情

EQUATION

反应方程式

HRID 1048617 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of aluminium chloride 4.71 g, sodium azide 6.89 g and tetrahydrofuran 100 mL was stirred with heating under reflux for one hour. After the reaction mixtures were cooled under ice-cooling, thereto were added a mixture of the above-mentioned 1-chloro-3-isocyanato-2-methylbenzene and tetrahydrofuran 10 mL and the resulting mixtures were stirred with heating under reflux for five hours. After cooling the mixtures, to a mixture of sodium nitrite 10.59 g and water 300 mL was added the reaction mixtures with stirring. The mixtures were acidified with concentrated hydrochloric acid and were extracted with ethyl acetate. The organic layers were dried over anhydrous sodium sulfate and were then concentrated under reduced pressure to give 1-(2-methyl-3-chlorophenyl)-1,4-dihydrotetrazole-5-one.

WORKUP

后处理

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