참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 1-Bromo-3-chlorobenzene | HCID 7928 | — |
| 반응물 | Tetrahydrofuran | HCID 8028 | — |
| 반응물 | 3-Piperidinone, 1-(phenylmethyl)- | HCID 96650 | — |
| 반응물 | Magnesium | HCID 5462224 | — |
| 용매 | Acetic Acid | HCID 176 | — |
| 생성물 | 3-(3-Chlorophenyl)-1-(phenylmethyl)-3-piperidinol hydrochloride | HCID 19095586 | 76% |
반응 단계
To a stirred and refluxed Grignard complex previously prepared starting from a mixture of 4.2 parts of 1-bromo-3-chlorobenzene, 5.4 parts of magnesium and 135 parts of tetrahydrofuran were added dropwise 19 parts of 1-(phenylmethyl)-3-piperidinone. Upon completion, stirring was continued for 1 hour at reflux temperature. After cooling, the reaction mixture was poured into ice water and 12.5 parts of acetic acid. The layers were separated. The aqueous phase was extracted with trichloromethane. The organic layer was washed with water, dried, filtered and evaporated. The residue was converted into the hydrochloride salt in 2-propanol. The salt was filtered off and dried, yielding 26 parts (76%) of 3-(3-chlorophenyl)-1-(phenylmethyl)-3-piperidinol hydrochloride (intermediate 27).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05001125 |
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| 출처 데이터셋 | uspto-grants-1991_03 |
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| ORD ID | ord-a077c131c37446cda95b2797740d3ca2 |
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| 출처 메모 | uspto-grants-1991_03 |
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