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Methane → 3-(2,2-Dimethylpropylideneamino)-pyrrolidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methane | HCID 297 | — |
| 反応物 | N,N'-Dibenzyl-3-aminopyrrolidine | HCID 14098325 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 3-(2,2-Dimethylpropylideneamino)-pyrrolidine | HCID 14836604 | 58% |
反応手順
36.8 g (0.138 mol) of 1-benzyl-3-benzylaminopyrrolidine are hydrogenated in 160 ml of methanol over 5 g of 5% strength palladium on active charcoal at 130° C. under a hydrogen pressure of 100 bar for 10 hours. The catalyst is filtered off and 16.6 g (0.138 mol ) of 71% strength pivalaldehyde are added to the filtrate, while stirring, after which the temperature rises from 20° C. to 28° C. The mixture is subsequently stirred for 30 minutes, the methanol is removed on a rotary evaporator and the residue is distilled. 12.7 g of 3-(2,2-dimethyl-propylidene-amino)-pyrrolidine of boiling point: 61° C./10 mbar are obtained with a purity, determined by gas chromatography, of 97%, corresponding to a yield of 58% of theory.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05723627 |
| 出典データセット | uspto-grants-1998_03 |
| ORD ID | ord-260f7eb07f4b4633acca339360195729 |
| 出典メモ | uspto-grants-1998_03 |