Reaktion #490747

Reaktionsgleichung

methyl 5-{[(tert-butoxycarbonyl)amino]methyl}-2-nitrobenzoate

ammonium formate

→

expected product

Ausbeute 81.1%

Methyl 2-amino-5-({[(1,1-dimethylethoxy)carbonyl]amino}methyl)benzoate

Ausbeute 81.1%

Lösungsmittel

EtOH

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeis irradiated under a microwave field at 120° C. for 5 min
2. 2
   FiltrationThe mixture is filtered
3. 3
   Sonstigethe filtrate is evaporated under reduced pressure
4. 4
   SonstigeThe residue is chromatographed on silica gel, elution

Vorschrift

A mixture of 0.273 g of methyl 5-{[(tert-butoxycarbonyl)amino]methyl}-2-nitrobenzoate, 0.166 g of ammonium formate and 0.094 g of Pd/C (10%) in 10 ml of EtOH purged beforehand with nitrogen is irradiated under a microwave field at 120° C. for 5 min. The mixture is filtered and the filtrate is evaporated under reduced pressure. The residue is chromatographed on silica gel, elution being carried out with an AcOEt/heptane mixture, (5/95, v/v) as far as (30/70, v/v), to give 0.2 g of the expected product.

Quelle