참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Tributylamine | HCID 7622 | — |
| 반응물 | Ethyl Acetate | HCID 8857 | — |
| 반응물 | 3,3-Diethoxy-1-propene | HCID 62477 | — |
| 반응물 | HCID 66691575 | HCID 66691575 | — |
| 촉매 | Tetrabutylammonium Chloride | HCID 70681 | — |
| 촉매 | palladium(II) acetate | HCID 167845 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | HCID 66691768 | HCID 66691768 | — |
반응 단계
To 1.80 g (5.17 mmol) 1-ethoxy-4-((4-iodophenyl)ethynyl)benzene (XII.1) in 24 mL DMF are added 2.36 mL (15.5 mmol) 3,3-diethoxy-propene, 3.69 mL (15.5 mmol) tributylamine, 1.44 g (5.17 mmol) tetrabutylammoniumchloride and 0.04 g (0.16 mmol) palladium(II)acetate under argon. The mixture is stirred at 120° C. for 12 h. After that time, 1.18 mL (7.76 mmol) 3,3-diethoxy-propene are added and the mixture is stirred at 120° C. for 5 d. After cooling, EtOAc is added and the mixture is washed with 1N potassium hydrogensulfate solution and water. The organic layer is dried over sodium sulphate and the solvent is evaporated. The residue is purified by column chromatography (silica gel; PE:DCM 1:1) to yield the desired product.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08877754B2 |
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| 출처 데이터셋 | uspto-grants-2014_11 |
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| ORD ID | ord-caeaae0a8b5941e9b57e00af235f045f |
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| 출처 메모 | uspto-grants-2014_11 |
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