関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Neopentyl glycol | HCID 31344 | — |
| 反応物 | 2-Bromo-1-(4-ethoxyphenyl)ethanone | HCID 2113060 | — |
| 反応物 | N,N-Bis(2-methylpropyl)prop-1-en-1-amine | HCID 54063094 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 3-(5,5-Dimethyl-1,3-dioxan-2-yl)-1-(4-ethoxyphenyl)butan-1-one | HCID 11722698 | 73.4% |
反応手順
2-Bromo-1-(4-ethoxyphenyl)ethan-1-one (4.0 g) and N,N-bis(2-methylpropyl)-1-propenylamine (4.0 g) were added to 16 ml of dimethylformamide under an atmosphere of nitrogen and the mixture was stirred between 50° C. and 55° C. for 2 hours. To the reaction mixture were added successively 1.6 g of paratoluenesulfonic acid and 2.1 g of neopentyl glycol and the mixture was stirred between 50° C. and 60° C. for 3 hours. After addition of 8 ml of water to the reaction mixture and cooling the reaction mixture to the room temperature, crystals precipitated. These crystals were isolated by filtration to give 3.7 g (yield 72%) of the title compound as white crystals. The 1H-NMR spectrum of the product is substantially identical with that of the product of Example 1.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07176323B2 |
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| 出典データセット | uspto-grants-2007_02 |
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| ORD ID | ord-73a82ee9d658472f99a72f6156eaee4e |
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| 出典メモ | uspto-grants-2007_02 |
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