反応 #4698

反応方程式

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

→

4-(3-ethyl-4-phenyl-4H-1,2,4-triazol-5-yl)-phenol

収率 88.5%

溶媒

hydrobromic acid

反応条件

後処理

1. 1
   その他the mixture was evaporated to dryness under reduced pressure
2. 2
   workup.DISSOLUTIONThe residue was dissolved in 20 ml of hot water
3. 3
   workup.ADDITIONammonium hydroxide was added until the pH
4. 4
   workup.WAITThe mixture was stood overnight
5. 5
   workup.STIRRINGwith stirring
6. 6
   洗浄The product was washed with water
7. 7
   その他dried at 90° C. under reduced pressure
8. 8
   その他The 3.65 g of product were crystallized from methanol
9. 9
   ろ過vacuum filtered
10. 10
    洗浄The crystals were washed
11. 11
    その他were dried at 90° C. under reduced pressure

実験手順

A solution of 3.86 g of 3-ethyl-5-(4-methoxyphenyl)-4-phenyl-4H-1,2,4-triazole and 20 ml of a hydrobromic acid solution at 48% was refluxed with stirring for one hour and the mixture was evaporated to dryness under reduced pressure. The residue was dissolved in 20 ml of hot water and ammonium hydroxide was added until the pH was alkaline. The mixture was stood overnight with stirring and was vacuum. The product was washed with water and dried at 90° C. under reduced pressure. The 3.65 g of product were crystallized from methanol and the mixture was iced and vacuum filtered. The crystals were washed by empasting with methanol and were dried at 90° C. under reduced pressure to obtain 3.245 g of 4-(3-ethyl-4-phenyl-4H-1,2,4-triazol-5-yl)-phenol melting at 275° C.

出典