反応 #64497

反応方程式

5-n-butyl-2,4-dihydro-4-[[2'-(N-trityltetrazol-5-yl)biphenyl-4-yl]methyl]-3H- 1,2,4-triazol-3-one

5-n-Butyl-2,4-dihydro-4-[[2'-(N-trityltetrazol-5-yl)biphenyl-4-yl]methyl]-3H-1,2,4-triazol-3-one

phenacyl bromide

→

desired compound

収率 81.0%

5-n-Butyl-2,4-dihydro-2-phenacyl-4-[[2'-(N-trityltetrazol-5-yl)biphenyl-4-yl]methyl]-3H-1,2,4-triazol-3-one

収率 81.0%

反応条件

後処理

1. 1
   その他chromatographed over silica gel (25 mL for 0.162 mmole, gradient elution using 0.5-2.0% MeOH/CH2Cl2)

実験手順

The alkylation of 5-n-butyl-2,4-dihydro-4-[[2'-(N-trityltetrazol-5-yl)biphenyl-4-yl]methyl]-3H- 1,2,4-triazol-3-one (from Example 2, Step D) with phenacyl bromide was carried out as described in Example 3, Step A, except that only 3 equivalents of the alkylating agent was used. After work-up, the residue was flash chromatographed over silica gel (25 mL for 0.162 mmole, gradient elution using 0.5-2.0% MeOH/CH2Cl2) to give the desired compound as a white foam in 81% yield, homogeneous by TLC in 2% MeOH/CH2Cl2, mass spectrum (FAB) 736 (M+1)+.

出典