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

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 pressuure. 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.

1. customthe mixture was evaporated to dryness under reduced pressuure
2. dissolutionThe residue was dissolved in 20 ml of hot water
3. additionammonium hydroxide was added until the pH
4. waitThe mixture was stood overnight
5. stirringwith stirring
6. washThe product was washed with water
7. customdried at 90° C. under reduced pressure
8. customThe 3.65 g of product were crystallized from methanol
9. filtrationvacuum filtered
10. washThe crystals were washed
11. customwere dried at 90° C. under reduced pressure

ORDレコード

ord-2962a2707aea4ca48be2dfcf6561c200

出典データセット

uspto-grants-1985_04

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US04512997