반응 #1135803

반응 방정식

sodium nitrite

aluminium chloride

sodium azide

tetrahydrofuran

3-bromo-2-methylbenzoic acid chloride

tetrahydrofuran

hydrochloric acid

→

1-(2-methyl-3-bromophenyl)-1.4-dihydrotetrazole-5-one

용매

water

반응 조건

후처리

1. 1
   온도with heating
2. 2
   온도under reflux for two hours
3. 3
   기타After the reaction mixtures
4. 4
   온도were cooled under ice-
5. 5
   온도cooling
6. 6
   workup.ADDITIONwas added
7. 7
   workup.STIRRINGthe resulting mixtures were stirred
8. 8
   온도with heating
9. 9
   온도under reflux for ten hours
10. 10
    온도After cooling the mixtures
11. 11
    workup.ADDITIONwas added
12. 12
    기타the reaction mixtures
13. 13
    workup.STIRRINGwith stirring
14. 14
    추출were then extracted with ethyl acetate
15. 15
    건조The organic layers were dried over anhydrous sodium sulfate
16. 16
    농축were then concentrated under reduced pressure

실험 절차

A mixture of aluminium chloride 181.0 g, sodium azide 265.0 g and tetrahydrofuran 30.0 mL was stirred with heating under reflux for two hours. After the reaction mixtures were cooled under ice-cooling, and thereto was added a mixture of the above-mentioned 3-bromo-2-methylbenzoic acid chloride and tetrahydrofuran 200 mL and the resulting mixtures were stirred with heating under reflux for ten hours. After cooling the mixtures, to a mixture of sodium nitrite 407 g and water 1,500 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 were then concentrated under reduced pressure to give 1-(2-methyl-3-bromophenyl)-1.4-dihydrotetrazole-5-one.

출처