반응 #353250

반응 방정식

2-[2-(4-bromophenyl)-1,1-dimethyl-2-oxoethyl]-2,4-dihydro-4-[4-[4-(4-hydroxyphenyl)-1-piperazinyl]phenyl]-3H-1,2,4-triazol-3-one

sodium tetrahydroborate

Acetic acid

→

(±)-2-[2-(4-bromophenyl)-2-hydroxy-1,1-dimethylethyl]-2,4-dihydro-4-[4-[4-(4-hydroxyphenyl)-1-piperazinyl]phenyl]-3H-1,2,4-triazol-3-one

수율 87.0%

용매

1,4-dioxane

methanol

water

water

반응 조건

후처리

1. 1
   기타Crystallization
2. 2
   기타resulted
3. 3
   workup.STIRRINGThe reaction mixture was stirred for 4 hours at room temperature
4. 4
   여과The precipitate was filtered off by suction (Buchner)
5. 5
   기타the solid was crystallized from 1-butanol
6. 6
   여과The precipitate was filtered off
7. 7
   기타dried

실험 절차

A mixture of 2-[2-(4-bromophenyl)-1,1-dimethyl-2-oxoethyl]-2,4-dihydro-4-[4-[4-(4-hydroxyphenyl)-1-piperazinyl]phenyl]-3H-1,2,4-triazol-3-one (0.009 mol) and sodium tetrahydroborate (0.025 mol) in 1,4-dioxane (100 ml), methanol (30 ml) and water (50 ml) was stirred overnight. Acetic acid (5 ml) was added, followed by addition of water (500 ml). Crystallization resulted. The reaction mixture was stirred for 4 hours at room temperature. The precipitate was filtered off by suction (Buchner) and the solid was crystallized from 1-butanol. The precipitate was filtered off and dried, yielding 4.4 g (87%) of (±)-2-[2-(4-bromophenyl)-2-hydroxy-1,1-dimethylethyl]-2,4-dihydro-4-[4-[4-(4-hydroxyphenyl)-1-piperazinyl]phenyl]-3H-1,2,4-triazol-3-one; mp. 224.5° C. (comp. 21).

출처