참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Ethanol | HCID 702 | — |
| 반응물 | Methanol | HCID 887 | — |
| 반응물 | CP-99994 | HCID 5311057 | — |
| 촉매 | HCID 178418390 | HCID 178418390 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | (2S,3S)-2-phenylpiperidin-3-amine | HCID 9812908 | — |
반응 단계
In a bottle were placed 9 g of 10% palladium-carbon, 180 ml of methanol, 275 ml of ethanol, 6.5 ml of concentrated hydrochloric acid and 9 g of the hydrochloride salt of (2S,3S)-3-(2-methoxybenzylamino)-2-phenylpiperidine. The mixture was shaken under hydrogen (40 p.s.i.) overnight, after which 9 g of additional catalyst were added to the system and the mixture was shaken under hydrogen for 1 day. The mixture was diluted with water (250 mL), filtered through diatomaceous earth (Celite (trademark)) and the Celite was rinsed well with water. The filtrate was concentrated to a volume of ca. 600-700 mL, made basic with concentrated aqueous sodium hydroxide and extracted with chloroform. The chloroform extracts were dried (sodium sulfate) and concentrated to obtain 4.4 g of the title compound as a colorless oil.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05721255 |
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| 출처 데이터셋 | uspto-grants-1998_02 |
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| ORD ID | ord-e32cb3f0ef0e44669df25f7b69588d8d |
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| 출처 메모 | uspto-grants-1998_02 |
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