Реакция #1563892

Уравнение реакции

Compound 25

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

potassium carbonate

diisopropyl(bromomethyl)phosphonate

→

solid

Выход 41.0%

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

Выход 41.0%

Растворители

MeCN

Условия реакции

Обработка

1. 1
   Концентрированиеthe reaction mixture was concentrated under reduced pressure
2. 2
   workup.ADDITIONThe crude residue was diluted by ethyl acetate (50 mL)
3. 3
   Промывкаwashed with water (2×10 mL)
4. 4
   СушкаThen it was dried over anhydrous Na2SO4
5. 5
   Фильтрацияfiltered
6. 6
   Концентрированиеconcentrated under reduced pressure
7. 7
   ДругоеThe residue was purified by silica gel column chromatography (1:4 v/v ethyl acetate/petroleum ether)

Методика

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).

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