反应 #1563892

反应方程式

Compound 25

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

potassium carbonate

diisopropyl(bromomethyl)phosphonate

→

solid

收率 41.0%

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

收率 41.0%

溶剂

MeCN

反应条件

后处理

1. 1
   浓缩the reaction mixture was concentrated under reduced pressure
2. 2
   workup.ADDITIONThe crude residue was diluted by ethyl acetate (50 mL)
3. 3
   洗涤washed with water (2×10 mL)
4. 4
   干燥Then it was dried over anhydrous Na2SO4
5. 5
   过滤filtered
6. 6
   浓缩concentrated under reduced pressure
7. 7
   其他The residue was purified by silica gel column chromatography (1:4 v/v ethyl acetate/petroleum ether)

实验过程

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).

来源