참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | N-Vinylacetamide | HCID 78875 | — |
| 반응물 | Phosphine, (1-methylethylidene)bis[diphenyl- | HCID 12091099 | — |
| 반응물 | Trifluoro-methanesulfonic acid 3-pentafluoroethyl-phenyl ester | HCID 59506217 | — |
| 촉매 | palladium(II) acetate | HCID 167845 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | N-[1-(3-Pentafluoroethyl-phenyl)-vinyl]-acetamide | HCID 59506293 | — |
반응 단계
To a solution of the crude product of step 1 (0.75 g, 2.2 mmol) in DMF (10 ml) was added N-vinylacetamide (0.37 g, 4.36 mmol), triethylamine (243 mg, 0.33 ml, 2.40 mmol), palladium acetate (20 mg, 4 mol %) and bis(diphenylphosphino)propane (40 mg, 0.1 mmol). The reaction mixture was heated for 30 min at 130° C. using microwaves. The red solution was diluted and washed with hydrochloric acid (1M, 2×15 ml) and sodium hydrogen carbonate (saturated, 20 ml). The organic phase was dried over sodium sulphate and evaporated. Purification of the crude product by silica gel chromatography using ethyl acetate/n-heptane (2:1) gave the desired product.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08143242B2 |
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| 출처 데이터셋 | uspto-grants-2012_03 |
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| ORD ID | ord-952ca0b47f1a49ef9fa38068bfe476a6 |
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| 출처 메모 | uspto-grants-2012_03 |
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