반응 #1135818

반응 방정식

sodium nitrite

aluminium chloride

sodium azide

tetrahydrofuran

3-trifluoromethyl-2-methylbenzoic acid chloride

tetrahydrofuran

hydrochloric acid

→

1-(2-methyl-3-trifluoromethylphenyl)-1,4-dihydrotetrazole-5-one

용매

water

반응 조건

후처리

1. 1
   온도with heating
2. 2
   온도under reflux for two hours
3. 3
   기타The reaction mixtures
4. 4
   온도were cooled under ice-
5. 5
   온도cooling
6. 6
   workup.STIRRINGthe mixtures were stirred
7. 7
   온도with heating
8. 8
   온도under reflux for ten hours
9. 9
   온도After cooling the mixtures
10. 10
    workup.ADDITIONwas added
11. 11
    기타the reaction mixtures
12. 12
    workup.STIRRINGwith stirring
13. 13
    추출were then extracted with ethyl acetate
14. 14
    건조The organic layers were dried over anhydrous sodium sulfate
15. 15
    농축the resulting mixtures were then concentrated under reduced pressure

실험 절차

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.

출처