تفاعل #69016

معادلة التفاعل

formamidine acetate

hydrazine hydrate

ethyl 2,2,2-trifluoroacetate

→

3-(Trifluoromethyl)-1H-1,2,4-triazole

المذيبات

EtOH

EtOH

ظروف التفاعل

المعالجة

1. 1
   تركيزconcentrated in vacuo
2. 2
   درجة الحرارةthe reaction was warmed
3. 3
   درجة الحرارةto reflux for 3 h
4. 4
   درجة الحرارةThe reaction was cooled
5. 5
   تركيزconcentrated in vacuo
6. 6
   غسيلwashed with sat. aq. NaHCO3 (2×)
7. 7
   تجفيفThe organic layer was dried (MgSO4)
8. 8
   تركيزconcentrated
9. 9
   أخرىto give a pale yellow oil which
10. 10
    أخرىwas used without further purification

الإجراء التجريبي

To a solution of hydrazine hydrate (2.7 mL, 48.6 mmol) in EtOH (80 mL) was added ethyl 2,2,2-trifluoroacetate (6.3 mL, 48.6 mmol). The reaction was aged at room temperature for 90 minutes and concentrated in vacuo. To the crude residue was added EtOH (50 mL) and formamidine acetate (5.1 g, 48.6 mmol) and the reaction was warmed to reflux for 3 h. The reaction was cooled, concentrated in vacuo, and taken up in EtOAc and washed with sat. aq. NaHCO3 (2×). The organic layer was dried (MgSO4) and concentrated to give a pale yellow oil which was used without further purification. 1H NMR (CDCl3, 400 MHz) δ 13.6 (br s, 1H), 8.5 (s, 1H).

المصدر