関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Formamide | HCID 713 | — |
| 反応物 | 2,2,4,4-Tetramethylthietan-3-one | HCID 282214 | — |
| 反応物 | AlCl3.6H2O | HCID 9794789 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 3-Amino-2,2,4,4-tetramethylthietane | HCID 11521099 | 60% |
反応手順
Formamide (8.0 g, 178 mmol), 2,2,4,4-tetramethyl-3-oxothietane (1.0 g, 6.933 mmol) and aluminum chloride hexahydrate (100 mg) were placed in a Teflon lined Parr bomb and heated at 170° C. for 18 hours. The reaction was then cooled and taken up in water (20 ml). The aqueous solution was extracted with methylene chloride (3×20 ml), the extracts combined and concentrated under reduced pressure. The residue was refluxed with 1N HCl (20 ml) for 4 hours, the reaction cooled and washed with methylene chloride (2×20 ml). It was then brought to pH 14 by addition of 6N sodium hydroxide and extracted with the methylene chloride (3×20 ml). The combined extracts were dried (Na2SO4) and concentrated to give 0.600 g (60%) of title product, verified by its 1H-NMR spectrum.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04851548 |
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| 出典データセット | uspto-grants-1989_07 |
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| ORD ID | ord-d3bd278feb8d4b478b4f07988b4c0c62 |
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| 出典メモ | uspto-grants-1989_07 |
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