참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Tetrahydrofuran | HCID 8028 | — |
| 반응물 | 4-Ethylresorcinol | HCID 17927 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | (Chloro(phenylmethoxy)phosphoryl)oxymethylbenzene | HCID 4641201 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | HCID 86682689 | HCID 86682689 | 84% |
반응 단계
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 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08486919B2 |
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| 출처 데이터셋 | uspto-grants-2013_07 |
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| ORD ID | ord-3b038dd0f79844eb9315b9354b832b37 |
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| 출처 메모 | uspto-grants-2013_07 |
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