참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | 4-Phenylpiperidine | HCID 69873 | — |
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 반응물 | 4-Bromo-2,2-diphenylbutyronitrile | HCID 96575 | — |
| 용매 | 2-Methoxyethanol | HCID 8019 | — |
| 생성물 | 2,2-Diphenyl-4-(4-phenylpiperidino)butyronitrile | HCID 21404797 | — |
반응 단계
A mixture of 18.6 parts of 2,2-diphenyl-4-bromobutyronitrile, 10.0 parts of 4-phenylpiperidine, 8.0 parts of N,N-diisopropylethylamine and 200 parts by volume of 2-methoxyethanol is heated at reflux for 16 hours. The solution is then cooled and stripped in vacuum. The resulting residue is partitioned between dilute sodium hydroxide and ether. Extraction of the ether phase with dilute hydrochloric acid results in the precipitation of an oil. This oil and the aqueous phase of the partitioning are combined, treated with aqueous sodium hydroxide and extracted with 1:1 ether-benzene mixture. The ether-benzene extract is dried over sodium sulfate and stripped in vacuum to give a solid. Crystallization of the solid from a mixture of skelly B and ether provided 2,2-diphenyl-4-(4-phenylpiperidino)butyronitrile, melting at 88° - 89.5° C. and having the following formula ##STR7##
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04053477 |
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| 출처 데이터셋 | uspto-grants-1977_10 |
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| ORD ID | ord-80f40e08ab6c4dbaa52aaa3b6f595c62 |
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| 출처 메모 | uspto-grants-1977_10 |
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