참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | P,P-Diphenylphosphinic azide | HCID 199401 | — |
| 반응물 | 1-(3,4,5-Trimethoxybenzoyl)piperazine | HCID 2874204 | — |
| 반응물 | HCID 67731480 | HCID 67731480 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | HCID 15230540 | HCID 15230540 | 86.4% |
반응 단계
1 ml of a methylene chloride solution containing 0.330 g of diphenylphosphoryl azide and then 0.280 g of 1-(3,4,5-trimethoxybenzoyl)piperazine were added to 5 ml of a methylene chloride solution containing both 0.224 g of (E)-3-phenyl-3-(4-pyridyl)acrylic acid (prepared as described in Preparation 3) and 0.28 ml of triethylamine. The mixture was then stirred for 4 hours at room temperature, after which the reaction solution was diluted with 20 ml of methylene chloride. It was then washed with a 5% w/v aqueous solution of sodium bicarbonate, followed by a saturated aqueous solution of sodium chloride, and the organic phase was dried over anhydrous sodium sulfate. The solvent was then removed by distillation under reduced pressure, and the oily residue (0.686 g) was purified by silica gel flash chromatography. 0.419 g of the title compound was obtained as a white powder from the fractions eluted with mixtures of methylene chloride and methanol ranging from 100:2 to 100:3 by volume.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05192766 |
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| 출처 데이터셋 | uspto-grants-1993_03 |
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| ORD ID | ord-7a72a9693ff34eccbefcfb9e01a688a1 |
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| 출처 메모 | uspto-grants-1993_03 |
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