Reaktion #2021768

Reaktionsgleichung

compound ( 28 )

[2-[4-[4-[4-[4-[[2-(2,4-difluorophenyl)-2-(1H-1,2,4-triazol-1-ylmethyl)-1,3-dioxolan-4-yl]methoxy]phenyl]-1-piperazinyl]phenyl]-4,5-dihydro-5-oxo-1H-1,2,4-triazol-1-yl]-1-methylpropyl]carbamate

NaHCO3

→

2-(2-amino-1-methylpropyl)-4-[4-[4-[4-[[2-(2,4-difluorophenyl)-2-(1H-1,2,4-triazol-1-ylmethyl)-1,3-dioxolan-4-yl]methoxy]phenyl]-1-piperazinyl]-phenyl]-2,4-dihydro-3H-1,2,4-triazol-3-one

Lösungsmittel

CF3COOH

CH2Cl2

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe organic layer was separated
2. 2
   Sonstigedried
3. 3
   Filtrationfiltered
4. 4
   Sonstigethe solvent was evaporated
5. 5
   SonstigeThe residue was triturated in 2-propanol
6. 6
   Filtrationfiltered off
7. 7
   Sonstigedried

Vorschrift

A mixture of compound (28)(0.0038 mol) in CF3COOH (10 ml) and CH2Cl2 (50 ml) was stirred at room temperature for 4 hours and neutralized with a NaHCO3 solution. The organic layer was separated, dried, filtered and the solvent was evaporated. The residue was triturated in 2-propanol, filtered off and dried, yielding 2.4 g (92%) of [2S-[2α,4α(S*,R*)]]-2-(2-amino-1-methylpropyl)-4-[4-[4-[4-[[2-(2,4-difluorophenyl)-2-(1H-1,2,4-triazol-1-ylmethyl)-1,3-dioxolan-4-yl]methoxy]phenyl]-1-piperazinyl]-phenyl]-2,4-dihydro-3H-1,2,4-triazol-3-one (compound 37; mp. 168.5° C.).

Quelle