참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | tert-Butyl acrylate | HCID 15458 | — |
| 반응물 | Tris(1,1-dimethylethyl)phosphine | HCID 83681 | — |
| 반응물 | Ethyl 2-(2-bromophenyl)acetate | HCID 2780092 | — |
| 반응물 | alpha-Cyclohexylcyclohexanemethanamine | HCID 10774245 | — |
| 촉매 | Bis(dibenzylideneacetone)palladium | HCID 9811564 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 용매 | 1,4-Dioxane | HCID 31275 | — |
| 생성물 | (E)-tert-Butyl 3-(2-(2-ethoxy-2-oxoethyl)phenyl)acrylate | HCID 86647801 | — |
반응 단계
To a mixture of ethyl 2-(2-bromophenyl)acetate (0.97 g, 4 mmol), t-butyl acrylate (0.51 g, 4 mmol), tris(dibenzylideneacetone)dipalladium(0) (91 mg, 0.1 mmol), dicyclohexylmethylamine (0.98 g, 5 mmol) in dioxane (5 mL) was added tri-tert-butylphosphine (0.2 mL, 1 N in toluene, 0.2 mmol). The mixture was heated at 70° C. for 30 minutes under N2. Ethyl acetate was added, and the mixture was filtered through diatomaceous earth. The filtrate was concentrated and purified by silica gel column chromatography eluting with hexanes and ethyl acetate (10:1) to afford the title compound. 1H NMR (300 MHz, DMSO-d6) δ ppm 7.79 (m, 1H), 7.72 (d, J=15.6 Hz, 1H), 7.34 (m, 3H), 6.40 (d, J=15.7 Hz, 1H), 4.06 (q, J=7.2 Hz, 2H), 3.84 (s, 2H), 1.48 (s, 9H), and 1.17 (t, J=2 Hz, 3H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09187483B2 |
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| 출처 데이터셋 | uspto-grants-2015_11 |
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| ORD ID | ord-0c4be9da58504281b6d0eeecc0498791 |
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| 출처 메모 | uspto-grants-2015_11 |
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