반응 #485951

반응 방정식

hydroxymethylphosphonic acid diethylester

1-chloro-2-chloromethyl-2-propene

tetrabutylammonium iodine

ammonium chloride

→

title product

(2-Chloromethyl-2-propenyloxymethyl)phosphonic acid diethylester

용매

tetrahydrofuran

sodium hydride

반응 조건

후처리

1. 1
   workup.ADDITIONis added (0.24 g, 6 mmol 60% in oil) at 0° C
2. 2
   추출extracted with ethyl acetate

실험 절차

To a mixture of hydroxymethylphosphonic acid diethylester (0.84 g, 5 mmol), 1-chloro-2-chloromethyl-2-propene (0.95 g, 7.6 mmol) and tetrabutylammonium iodine (0.18 g, 0.5 mmol) in anhydrous tetrahydrofuran (10 ml), sodium hydride is added (0.24 g, 6 mmol 60% in oil) at 0° C. The mixture is stirred overnight at 20° C. The reaction mixture is hydrolyzed with a saturated solution of ammonium chloride, extracted with ethyl acetate and the title product is obtained by flash chromatography on silica gel (0.35 g, 27%).

출처