Hydrochloric Acid → HCID 13269992, compound

Participants

Reaction Conditions

Reaction Steps

22.9 g (0.06 mol) of 1-(2,4-dichlorophenyl)-2-(1,2,4-triazol-1-yl)-4-(dioxolan-2-yl)-4-methyl-pentan-3-one are dissolved in 100 ml of methanol, the solution is cooled to 0° C., and 2.95 g (0.078 mol) of sodium borohydride are added in portions. The mixture is stirred for a further 3 hours at room temperature, 15 ml of concentrated hydrochloric acid are added dropwise, stirring is continued for a further 3 hours and 500 ml of saturated sodium bicarbonate solution are then added. The mixture is extracted with 400 ml of methylene chloride, the phases are separated, the organic phase is wshed with twice 100 ml of water, and the solvent is distilled off. The residue is taken up in 150 ml of diisopropyl ether, and the crystals are filtered off under suction. 1-(2,4-Dichlorophenyl)-2-(1,2,4-triazol-1-yl)-4-(dioxolan-2-yl)-4-methyl-pentan-3-ol is obtained as the B form of melting point 178°-81° C., and after approximately 100 ml of diisopropyl ether have been distilled off, 8.9 g of product are obtained as the A form of melting point 95°-100° C.

Provenance & Evidence