反応 #630058

反応方程式

3,4-bis-(4-methoxyphenyl)-5-ethyl-4H-1,2,4-triazole

hydrobromic acid

→

4,4'-(3-ethyl-4H-1,2,4-triazol-4,5-diyl)-bis-phenol

収率 80.6%

反応条件

後処理

1. 1
   workup.DISTILLATIONthe hydrobromic acid was distilled under reduced pressure
2. 2
   workup.DISSOLUTIONThe crystalline residue was dissolved in 30 ml of hot water
3. 3
   workup.ADDITIONammonium hydroxide was added
4. 4
   workup.WAITThe mixture stood overnight
5. 5
   workup.STIRRINGwith stirring
6. 6
   ろ過filtered
7. 7
   洗浄The product was washed with water
8. 8
   その他dried at 90° C. under reduced pressure
9. 9
   その他to obtain a product which
10. 10
    その他was crystallized from dimethylformamide
11. 11
    workup.WAITThe mixture was iced for one hour
12. 12
    ろ過filtered
13. 13
    洗浄The product was washed with a 3-4 dimethylformamide-water mixture
14. 14
    その他dried

実験手順

A solution of 6 g of 3,4-bis-(4-methoxyphenyl)-5-ethyl-4H-1,2,4-triazole and 25 ml of a solution of hydrobromic acid at 48% was refluxed with stirring for one hour and the hydrobromic acid was distilled under reduced pressure. The crystalline residue was dissolved in 30 ml of hot water and ammonium hydroxide was added thereto until the pH was alkaline. The mixture stood overnight with stirring and was vacuum filtered. The product was washed with water and dried at 90° C. under reduced pressure to obtain a product which was crystallized from dimethylformamide. The mixture was iced for one hour and was vacuum filtered. The product was washed with a 3-4 dimethylformamide-water mixture and dried to obtain 4.395 g of 4,4'-(3-ethyl-4H-1,2,4-triazol-4,5-diyl)-bis-phenol melting at 317°-318° C.

出典