반응 #536970

반응 방정식

dibenzyl chlorophosphate

tetrahydrofuran

4-cyclohexylresorcinol

sodium hydride

→

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

수율 64.0%

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 (20 ml)
4. 4
   건조dried with anhydrous sodium sulfate
5. 5
   농축concentrated

실험 절차

To a tetrahydrofuran solution (10 ml) of 4-cyclohexylresorcinol (926 mg), sodium hydride (60% dispersion in liquid paraffin) (404 mg) was added and stirred at 0° C. for 30 minutes. Then, dibenzyl chlorophosphate (10 w/v % solution in benzene) (30 ml) was added dropwise. After stirring at room temperature for 3 hours, water (30 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 (20 ml), dried with anhydrous sodium sulfate and then concentrated. The residue (4.12 g) was subjected to silica gel chromatography (silica gel 90 g, chloroform to chloroform:methanol=100:1), to give 1,3-bis(dibenzylphosphonooxy)-4-cyclohexylbenzene (2.19 g, yield: 64%) as a yellow liquid.

출처