関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2,6-Dibromopyridine | HCID 12274 | — |
| 反応物 | 4,4,N-Trimethoxy-N-methylbutyramide | HCID 59788083 | — |
| 反応物 | Butyllithium | HCID 178418339 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | n-[1-Eth-(z)-ylidene-5,5-dimethoxy-2-oxo-pentyl]acrylimidoyl bromide | HCID 87233323 | 74.9% |
反応手順
To a suspension of 2,6-dibromopyridine(8.1 g, 34.03 mmol) in 80 mL of ether at −70° C., is added BuLi(12.3 mL, 26.17 mmol, 2.5 M in Hexane) in on portion. After stirring at −70° C. for 5 min, 4,4,N-Trimethoxy-N-methyl-butyramide(5.0 g, 26.17 mmol) is added to the solution dropwise. After stirring at −70° C. for 1.5 hr, the reaction mixture is quenched with 120 mL of water and extracted with 3×130 mL of EtOAc. The combined organic layers is concentrated and purified by chromatography(Hexane/EtOAc:70/30) to give N-[1-Eth-(Z)-ylidene-5,5-dimethoxy-2-oxo-pentyl]-acrylimidoyl bromide(5.96 g, 60.5%) as light yellow liquid. M/Z=288.0
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07419975B2 |
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| 出典データセット | uspto-grants-2008_09 |
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| ORD ID | ord-4fd606995a9a445d89b0c7983409a85d |
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| 出典メモ | uspto-grants-2008_09 |
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