반응 #1563892

반응 방정식

Compound 25

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

potassium carbonate

diisopropyl(bromomethyl)phosphonate

→

solid

수율 41.0%

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

수율 41.0%

용매

MeCN

반응 조건

후처리

1. 1
   농축the reaction mixture was concentrated under reduced pressure
2. 2
   workup.ADDITIONThe crude residue was diluted by ethyl acetate (50 mL)
3. 3
   세척washed with water (2×10 mL)
4. 4
   건조Then it was dried over anhydrous Na2SO4
5. 5
   여과filtered
6. 6
   농축concentrated under reduced pressure
7. 7
   기타The residue was purified by silica gel column chromatography (1:4 v/v ethyl acetate/petroleum ether)

실험 절차

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).

출처