참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Ethanol | HCID 702 | — |
| 반응물 | 2-Phenylpropionitrile | HCID 15761 | — |
| 반응물 | HCID 178418361 | HCID 178418361 | — |
| 용매 | tert-Butyl methyl ether | HCID 15413 | — |
| 생성물 | 2-Phenylpropylamine hydrochloride | HCID 89332 | 76.2% |
반응 단계
Charge to an autoclave hydrogenation apparatus under nitrogen water-wet 5% palladium on carbon (453 g), ethanol (6.36 L), 2-phenylpropionitrile (636 g, 4.85 moles) and finally concentrated (12M) hydrochloric acid (613 g, 5.6 mole). Stir the mixture rapidly and pressurize to 75 to 78 psi with hydrogen. Heat the mixture 50° C. to 64° C. for 3 hours. Depressurize and filter the reaction mixture to afford two lots of filtrate. Concentrate filtrates under reduced pressure to approximately 400 mL each. Add methyl tert-butyl ether (MTBE) (2.2 L each) to each lot. Stir the precipitate overnight. Filter and wash solids with fresh MTBE (100 mL) and dry overnight. Combine the lots to afford 2-phenyl-1-propylamine HCl (634.4 g, 76.2%) as a white powder.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08097652B2 |
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| 출처 데이터셋 | uspto-grants-2012_01 |
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| ORD ID | ord-dc753b3f3cf94d54bf0285b696229e54 |
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| 출처 메모 | uspto-grants-2012_01 |
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