반응 #64496

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

tetrazole

→

desired compound

수율 43.0%

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

수율 43.0%

용매

CH2Cl2

반응 조건

후처리

1. 1
   기타flash chromatographed over silica gel (15 mL
2. 2
   세척for 0.19 mmole, gradient elution

실험 절차

The conversion of 5-n-butyl-2,4-dihydro-2-[1-(N-methylcarbamoyl)ethyl]-4-[(2'-cyanobiphenyl-4-yl)methyl]-3H-1,2,4-triazol-3-one to the corresponding tetrazole was accomplished by the procedure of Example 9, Step E, except that the mixture was stirred at 120° C. for 2 days. After work-up, the residue was taken up in CH2Cl2 and flash chromatographed over silica gel (15 mL for 0.19 mmole, gradient elution using 5-30% MeOH/CH2Cl2 to give the desired compound as a white powder in 43% yield, homogeneous by TLC in 30% MeOH/CH2Cl2, mass spectrum (FAB) 461 (M+1)+, mp 153°-155° C.

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