Reaktion #64563

Reaktionsgleichung

4-(4-bromo-2-fluorobenzyl)-5-n-butyl-2-[2-chloro-5-(methoxycarbonyl)phenyl]-2,4-dihydro-3H-1,2,4-triazol-3-one

4-(4-Bromo-2-fluorobenzyl)-5-n-butyl-2-[2-chloro-5-(methoxycarbonyl)phenyl]-2,4-dihydro-3H-1,2,4-triazol-3-one

CH2Cl2

MeOH

→

4-(4-Bromo-2-fluorobenzyl)-5-n-butyl-2-[5-(N-n-butylcarbamoyl)-2-chloro-phenyl]-2,4-dihydro-3H-1,2,4-triazol-3-one

Lösungsmittel

n-butylamine

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeevaporated in vacuo
2. 2
   Sonstigechromatographed on 15 cc of silica gel (gradient elution with 1-5% MeOH in CH2Cl2)
3. 3
   Sonstigeto yield 41 mg (76%) of colorless, glassy solid, mp 114°-116° C.

Vorschrift

A solution of 50 mg (0.10 mmole) of 4-(4-bromo-2-fluorobenzyl)-5-n-butyl-2-[2-chloro-5-(methoxycarbonyl)phenyl]-2,4-dihydro-3H-1,2,4-triazol-3-one (from Step D) in 1 mL of n-butylamine was stirred overnight at 65° C. and then evaporated in vacuo. The residue was flash chromatographed on 15 cc of silica gel (gradient elution with 1-5% MeOH in CH2Cl2) to yield 41 mg (76%) of colorless, glassy solid, mp 114°-116° C.; homogeneous by TLC (95:5 CH2Cl2 --MeOH); mass spectrum (FAB) m/e 537, 539 (M+1)+.

Quelle