関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | p-Toluenesulfonic acid | HCID 6101 | — |
| 反応物 | Neopentyl glycol | HCID 31344 | — |
| 反応物 | 2-Bromo-1-(3,4-dimethylphenyl)ethan-1-one | HCID 3703113 | — |
| 反応物 | N,N-Bis(2-methylpropyl)prop-1-en-1-amine | HCID 54063094 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 3-(5,5-Dimethyl-1,3-dioxan-2-yl)-1-(3,4-dimethylphenyl)butan-1-one | HCID 11449161 | 84% |
反応手順
2-Bromo-1-(3,4-dimethylphenyl)ethan-1-one (6.2 g) and N,N-bis(2-methylpropyl)-1-propenylamine (6.8 g) were added to 25 ml of acetonitrile under an atmosphere of nitrogen and the mixture was stirred at around 50° C. for 4 hours. After cooling the reaction mixture to 10° C., 25 ml of water, 4.3 g of neopentyl glycol, 6.2 g of concentrated sulfuric acid and 0.62 g of para-toluenesulfonic acid were added to the reaction mixture and the mixture was stirred at around 60° C. for 1 hour. After cooling the reaction mixture to the room temperature, crystals precipitated. These crystals were isolated by filtration to give 6.6 g (yield 84%) of the title compound as white crystals.
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-cbd65fef08cb4daebb6573b9e8ea563d |
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| 出典メモ | uspto-grants-2007_02 |
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