참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Benzonitrile, 4-bromo- | HCID 12162 | — |
| 반응물 | Ammonium Chloride | HCID 25517 | — |
| 반응물 | 4-chloro-N-methylpiperidine | HCID 79342 | — |
| 반응물 | Magnesium | HCID 5462224 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | (4-Bromophenyl)-(1-methyl-4-piperidinyl)methanone | HCID 20530733 | — |
반응 단계
To a stirred and cooled (10°-15° C.) Grignard-complex, previously prepared starting from 13.5 parts of 4-chloro-1-methylpiperidine and 2.4 parts of magnesium in 68 parts of tetrahydrofuran, is added dropwise a solution of 10 parts of 4-bromobenzonitrile in 22 parts of tetrahydrofuran. Upon completion, stirring is continued for 1 hour at reflux temperature. The reaction mixture is decomposed by pouring onto a mixture of 50 parts of ammonium chloride in 250 parts of water. The product is extracted with methylbenzene. The extract is dried, filtered and evaporated. The residue is purified by column-chromatography over silica gel using a mixture of trichloromethane and methanol (95:5 by volume) as eluent. The pure fractions are collected and the eluent is evaporated, yielding 10 parts of (4-bromophenyl)-(1-methyl-4-piperidinyl)methanone as a residue.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04342870 |
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| 출처 데이터셋 | uspto-grants-1982_08 |
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| ORD ID | ord-93eec3e9667745f9b5688539be76b279 |
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| 출처 메모 | uspto-grants-1982_08 |
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