반응 #536966

반응 방정식

dibenzyl chlorophosphate

tetrahydrofuran

4-ethylresorcinol

sodium hydride

→

1,3-bis(dibenzylphosphonooxy)-4-ethylbenzene

수율 84.0%

용매

water

반응 조건

후처리

1. 1
   workup.STIRRINGAfter stirring at room temperature for 3 hours
2. 2
   추출the extraction
3. 3
   세척Then, the extract was washed with saturated brine (10 ml)
4. 4
   건조dried with anhydrous sodium sulfate
5. 5
   농축concentrated

실험 절차

To a tetrahydrofuran solution (10 ml) of 4-ethylresorcinol (423 mg), sodium hydride (60% dispersion in liquid paraffin) (269 mg) was added and stirred at 0° C. for 30 minutes. Then, dibenzyl chlorophosphate (10 w/v % solution in benzene) (20 ml) was added dropwise. After stirring at room temperature for 3 hours, water (10 ml) was added to the reaction mixture, and the extraction was carried out with ethyl acetate (30 ml). Then, the extract was washed with saturated brine (10 ml), dried with anhydrous sodium sulfate and then concentrated. The residue (2.16 g) was subjected to silica gel chromatography (silica gel 60 g, chloroform to chloroform:methanol=50:1), to give 1,3-bis(dibenzylphosphonooxy)-4-ethylbenzene (1.65 g, yield: 84%) as a yellow liquid.

출처