関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 1-Isopropyl-3,3,5,5-tetramethyl-2-piperazinone | HCID 12580992 | — |
| 反応物 | Aluminium lithium hydride | HCID 21226445 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 1-Isopropyl-3,3,5,5-tetramethylpiperazine | HCID 23044987 | — |
反応手順
3.9 g (0.103 mol) of lithiumaluminium hydride are introduced into 100 ml of anhydrous tetrahydrofuran under a nitrogen atmosphere, while stirring and cooling. A solution of 19.8 g (0.1 mol) of 1-isopropyl-3,3,5,5-tetramethyl-2-piperazinone (obtainable, for example, in accordance with Synthesis 1981, page 40, or J. Organ. Chem., 45 (1980), 754-59) in 75 ml of anhydrous tetrahydrofuran is added dropwise at room temperature, whereupon the reaction temperature rises to 6020 C. The mixture is then stirred overnight at room temperature. After dropwise addition of about 10 ml of water, the mixture is subsequently stirred for 2 hours and the precipitate is then filtered off with suction. The filtrate is dried over potassium carbonate and concentrated in vacuo and the crude product which remains as a colourless oil is further processed without additional purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04937244 |
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| 出典データセット | uspto-grants-1990_06 |
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| ORD ID | ord-11165a5f4cae45b59dbfde76896cfbe6 |
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| 出典メモ | uspto-grants-1990_06 |
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