関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 4-Bromo-2,6-dimethylphenol | HCID 16919 | — |
| 反応物 | 1,7-Dibromoheptane | HCID 78309 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 5-Bromo-2-(7-bromoheptyloxy)-1,3-dimethylbenzene | HCID 22494636 | — |
反応手順
A solution of 4-bromo-2,6-dimethylphenol (2.00 g) and 1,7-dibromoheptane (5.10 g) in N,N-dimethylformamide (20 ml) was treated with potassium carbonate (2.06 g), and the mixture was stirred for 5 hours at ambient temperature. To the reaction mixture was added water and methylene chloride, and the organic layer was separated and dried over magnesium sulfate. Magnesium sulfate was filtered off, and the filtrate was concentrated in vacuo. The residue was purified by silica gel column chromatography eluting successively with the following solvents: (1) n-hexane, (2) n-hexane:ethyl acetate=4:1, (3) n-hexane:ethyl acetate=1:1. The fractions containing the object compound were concentrated in vacuo to give crude 5-bromo-2-(7-bromoheptyloxy)-1,3-dimethylbenzene, that was used in the next reaction directly, as a pale yellow oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06884868B1 |
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| 出典データセット | uspto-grants-2005_04 |
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| ORD ID | ord-7fc2b0d85ff048f1a19a243b72b12415 |
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| 出典メモ | uspto-grants-2005_04 |
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