참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Pivalaldehyde | HCID 12417 | — |
| 반응물 | 3-Aminopyrrolidine | HCID 164401 | — |
| 용매 | Toluene | HCID 1140 | — |
| 생성물 | 3-(2,2-Dimethylpropylideneamino)-pyrrolidine | HCID 14836604 | 74% |
반응 단계
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).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05723627 |
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| 출처 데이터셋 | uspto-grants-1998_03 |
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| ORD ID | ord-c0f745d78785401496f0649633321e35 |
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| 출처 메모 | uspto-grants-1998_03 |
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