Hydrochloric Acid → HCID 20070436, compound

Participants

Reaction Steps

While stirring and passing a current of nitrogen through the reaction mixture, 0.56 g (14.7 mmol) of sodium borohydride is added in portions at room temperature and within a period of 15 minutes to a solution of 5.8 g (14.7 mmol) of 2-[4-(4-bromophenoxy)-2-chlorophenyl]-1-(1H-1,2,4-triazol-1-yl)-ethan-2-one in 40 ml of methanol. The temperature of the reaction mixture rises from 22° to 38°. When the addition is complete, stirring is continued for a further 4 hours at room temperature and then 2.2 g of concentrated hydrochloric acid are added, followed somewhat later by the addition of 22 ml of 10% sodium hydrogen carbonate solution. The title compound is precipitated in crystalline form. It is isolated by filtration, washed with water and dried, to give 5.5 g of 2-[4-(4-bromophenoxy)-2-chlorophenyl]-1-(1H-1,2,4-triazol-1-yl)-ethan-2-ol om the form of a beige crystalline powder. Melting point 115°-118° C.

Provenance & Evidence