Hydrochloric Acid → 3,3-Bisfluoromethyl-1-(4-chlorophenoxy)-1-(1,2,4-triazol-1-yl)-butan-2-ol

反応式

[F:1][CH2:2][C:3]([CH2:21][F:22])([CH3:20])[C:4](=[O:19])[CH:5]([O:11][C:12]1[CH:17]=[CH:16][C:15]([Cl:18])=[CH:14][CH:13]=1)[N:6]1[CH:10]=[N:9][CH:8]=[N:7]1.[BH4-].[Na+].Cl>CO>[F:1][CH2:2][C:3]([CH2:21][F:22])([CH3:20])[CH:4]([OH:19])[CH:5]([O:11][C:12]1[CH:17]=[CH:16][C:15]([Cl:18])=[CH:14][CH:13]=1)[N:6]1[CH:10]=[N:9][CH:8]=[N:7]1

参加物

実験手順

130.5 g (0.395 mol) of 3,3-bisfluoromethyl-1-(4-chlorophenoxy)-1-(1,2,4-triazol-1-yl)-2-butanone were dissolved in 800 ml of methanol, and 21 g (0.55 mol) of sodium borohydride were added in portions. The reaction solution was subsequently stirred for 15 hours and was then adjusted to a pH value of 3 with concentrated hydrochloric acid. The mixture was then stirred for 2 hours. After distilling off the solvent in vacuo, water/sodium bicarbonate were added to the residue and the mixture was extracted by shaking with 600 ml of methylene chloride. The combined organic phases were dried over sodium sulphate and concentrated in vacuo. The residue was crystallized with diisopropyl ether. 112 g (86% of theory) of 3,3-bisfluoromethyl-1-(4-chlorophenoxy)-1-(1,2,4-triazol-1-yl)-butan-2-ol of melting point 97°-102° C. were obtained. ##STR77##