関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 4-Chlorophenol | HCID 4684 | — |
| 反応物 | 2,6-Dimethyl-1,4-benzoquinone | HCID 68241 | — |
| 反応物 | (2-Methyl-pent-4-en-2-oxy)diphenylphosphine | HCID 59173107 | — |
| 溶媒 | 1,1-Dichloroethane | HCID 6365 | — |
| 生成物 | 1-Chloro-4-(1,1-dimethyl-but-3-enyloxy)-benzene | HCID 20357190 | 2% |
反応手順
To a cooled (0° C.), stirred mixture of 4-chloro-phenol (4.34 g) and 2,6-dimethylbenzoquinone (4.60 g) was added dropwise a solution of (2-methyl-pent-4-en-2-oxy)diphenylphosphine (8.0 g) in dichloroethane (20 ml). The mixture was then heated at 95° C. for 24 h. The reaction mixture was cooled to room temperature and concentrated in vacuo and the residue was purified by column chromatography (SiO2; gradient: heptane/EtOAc) to give 1-chloro-4-(1,1-dimethyl-but-3-enyloxy)-benzene (0.14 g, 2%) as a colourless oil. MS (EI): 171.1 ([{37Cl}M−C3H5−]+), 1691 ([{35Cl}M−C3H5]+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08242153B2 |
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| 出典データセット | uspto-grants-2012_08 |
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| ORD ID | ord-c15e42ad2639456eb37993d3fe98a7f6 |
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| 出典メモ | uspto-grants-2012_08 |
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