참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | 1-benzyl-N-methyl-5-oxopyrrolidine-3-carboxamide | HCID 13491794 | — |
| 반응물 | Aluminium lithium hydride | HCID 21226445 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 1-(1-benzylpyrrolidin-3-yl)-N-methylmethanamine | HCID 4660832 | 88.5% |
반응 단계
To a suspension of 37.40 g (1.00 mole) lithium aluminum hydride in 1000 ml tetrahydrofuran, was added a solution of 88.3 g (0.380 mole) of N-methyl-5-oxo-1-(phenylmethyl)-3-pyrrolidinecarboxamide in tetrafuran dropwise under nitrogen. The reaction was then refluxed overnight. The reaction flask was cooled in an ice bath and 37.4 ml of water, 37.4 ml of 15% sodium hydroxide and 112.2 ml of water were added. The precipitated solids were filtered and washed with hot ethanol. The combined filtrates were concentrated, then dissolved in dichloromethane, filtered, dried over magnesium sulfate, and the solvent evaporated under reduced pressure to give 68.68 g of N-methyl-1-(phenylmethyl)-3-pyrrolidinemethanamine as an oil. This material was used without further purification in the next step.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04604401 |
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| 출처 데이터셋 | uspto-grants-1986_08 |
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| ORD ID | ord-69cb13b5f8eb403dbc010d76bedf76ae |
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| 출처 메모 | uspto-grants-1986_08 |
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