Reaktion #1563892

Reaktionsgleichung

Compound 25

2-amino-N-(2-methoxyphenyl)-6-(4-nitrophenylthi-o)benzamide

potassium carbonate

diisopropyl(bromomethyl)phosphonate

→

solid

Ausbeute 41.0%

diisopropyl(((2-((2-methoxyphenyl)carbamoyl)-3-((4-nitro-phenyl)thio)phenyl)amino)methyl)phosphonate

Ausbeute 41.0%

Lösungsmittel

MeCN

Reaktionsbedingungen

Aufarbeitung

1. 1
   Einengenthe reaction mixture was concentrated under reduced pressure
2. 2
   workup.ADDITIONThe crude residue was diluted by ethyl acetate (50 mL)
3. 3
   Waschenwashed with water (2×10 mL)
4. 4
   TrocknenThen it was dried over anhydrous Na2SO4
5. 5
   Filtrationfiltered
6. 6
   Einengenconcentrated under reduced pressure
7. 7
   SonstigeThe residue was purified by silica gel column chromatography (1:4 v/v ethyl acetate/petroleum ether)

Vorschrift

Compound 25 (1.0 equiv.) was dissolved in MeCN (40 mL) and treated with anhydrous potassium carbonate (2.0 equiv.) at room temperature. To this mixture diisopropyl(bromomethyl)phosphonate (1.2 equiv.) was added via a micro syringe. After being stirred for 4 Hours at 60° C., the reaction mixture was concentrated under reduced pressure. The crude residue was diluted by ethyl acetate (50 mL), and washed with water (2×10 mL). Then it was dried over anhydrous Na2SO4, filtered, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (1:4 v/v ethyl acetate/petroleum ether) to provide a yellow solid (235.2 mg, 41% yield).

Quelle