참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | Sulfuric acid magnesium salt (1:1) | HCID 24083 | — |
| 반응물 | Ethyl 1-butylpiperidine-4-carboxylate | HCID 9990801 | — |
| 반응물 | 1-n-Butylisonipecotic acid | HCID 17892696 | — |
| 반응물 | Aluminium lithium hydride | HCID 21226445 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | (1-Butylpiperidin-4-yl)methanol | HCID 10241250 | 115.2% |
반응 단계
A suspension of lithium aluminum hydride (1.39 g) in THF (100 ml) was ice-cooled, to which was added dropwise a solution of a mixture (4.15 g) of ethyl 1-n-butylisonipecotate and 1-n-butylisonipecotic acid obtained in Preparation Example 19 in THF (100 ml) over a period of 15 minutes with stirring. The mixture was stirred under ice-cooling for 10 minutes, and then at room temperature for 30 minutes. To the reaction solution were successively added water (2 ml), a 15% aqueous solution of sodium hydroxide (2 ml), water (6 ml) and anhydrous magnesium sulfate, and the mixture was stirred at room temperature for 30 minutes. The reaction solution was filtered off with Celite, and the solvent was distilled off under reduced pressure to give the title compound (3.84 g). This compound was used for the subsequent reaction without purification.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05945434 |
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| 출처 데이터셋 | uspto-grants-1999_08 |
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| ORD ID | ord-db8a2d6b75414c988dc0505196928f4f |
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| 출처 메모 | uspto-grants-1999_08 |
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