참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Triphenylphosphine | HCID 11776 | — |
| 반응물 | 3-(3,4-Dichlorophenyl)propan-1-ol | HCID 19075313 | — |
| 반응물 | Diethylazodicarboxylate toluene | HCID 66777355 | — |
| 반응물 | Ethyl 3-ethoxy-3-(4-hydroxyphenyl)propionate | HCID 67058135 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | Ethyl 3-{4-[3-(3,4-dichlorophenyl)propoxy]phenyl}-3-ethoxypropionate | HCID 67058188 | 73% |
반응 단계
Ethyl 3-ethoxy-3-(4-hydroxyphenyl)propionate (100 mg, 0.420 mmol) produced in Example 1 (1C) and 3-(3,4-dichlorophenyl)propanol (129 mg, 0.630 mmol) synthesized in (11A) were dissolved in tetrahydrofuran (10 mL), and triphenylphosphine (178 mg, 0.680 mmol) and a 40% diethyl azodicarboxylate toluene solution (309 μL, 0.680 mmol) were added thereto at room temperature, and then, the resulting mixture was stirred under a nitrogen atmosphere at 50° C. for 4 hours. After the reaction solution was cooled to room temperature, the solvent was distilled off under reduced pressure, and the resulting residue was purified by silica gel column chromatography (hexane:ethyl acetate=100:0 to 95:5 (v/v)), whereby the objective title compound was obtained as a colorless oily substance (130 mg, yield: 73%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08222281B2 |
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| 출처 데이터셋 | uspto-grants-2012_07 |
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| ORD ID | ord-5d20314ba4d54297a24e199902750b6d |
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| 출처 메모 | uspto-grants-2012_07 |
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