関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Pivalaldehyde | HCID 12417 | — |
| 反応物 | 3-Aminopyrrolidine | HCID 164401 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 3-(2,2-Dimethylpropylideneamino)-pyrrolidine | HCID 14836604 | 74% |
反応手順
34.5 g (0.4 mol) of 3-aminopyrrolidine are initially introduced into 100 ml of toluene, and 34.5 g (0.3 mol) of 75% strength pivalaldehyde (preparation from Riedel-de-Haen) in 100 ml of toluene are added dropwise at 20° C., while cooling in a water bath. The mixture is subsequently stirred at room temperature for 2 hours, the aqueous phase is then separated off in a separating funnel (4.6 ml) and the toluene solution is dried over sodium sulphate for 1 hour. The toluene is separated off on a rotary evaporator and the residue is distilled using a small Vigreux column. 46.2 g of 3-(2,2-dimethylpropylideneamino)-pyrrolidine of boiling point 61° C./10 mbar are obtained with a purity, determined by gas chromatography, of 98%, corresponding to a yield of 74% and a selectivity of 99% (pivalaldehyde).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05648493 |
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| 出典データセット | uspto-grants-1997_07 |
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| ORD ID | ord-4c1a66e4a85044c985a27efcecdb09d2 |
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| 出典メモ | uspto-grants-1997_07 |
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