تفاعل #1135818

معادلة التفاعل

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

المذيبات

water

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةwith heating
2. 2
   درجة الحرارةunder reflux for two hours
3. 3
   أخرىThe reaction mixtures
4. 4
   درجة الحرارةwere cooled under ice-
5. 5
   درجة الحرارةcooling
6. 6
   workup.STIRRINGthe mixtures were stirred
7. 7
   درجة الحرارةwith heating
8. 8
   درجة الحرارةunder reflux for ten hours
9. 9
   درجة الحرارةAfter cooling the mixtures
10. 10
    workup.ADDITIONwas added
11. 11
    أخرىthe reaction mixtures
12. 12
    workup.STIRRINGwith stirring
13. 13
    استخلاصwere then extracted with ethyl acetate
14. 14
    تجفيفThe organic layers were dried over anhydrous sodium sulfate
15. 15
    تركيزthe resulting mixtures were then concentrated under reduced pressure

الإجراء التجريبي

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.

المصدر