참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | Ammonium Chloride | HCID 25517 | — |
| 반응물 | 4,6-Dichloro-5-fluoropyrimidine | HCID 11286675 | — |
| 반응물 | 2,5-dimethylhexahydro-1H-azepine hydrochloride | HCID 66594832 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 생성물 | 1-(6-chloro-5-fluoro pyrimidin-4-yl)-2,5-dimethylhexahydro-1H-azepine | HCID 59341137 | 97.2% |
반응 단계
Into 3 ml of acetonitrile were added 0.2 g of 4,6-dichloro-5-fluoropyrimidine, 0.50 g of potassium carbonate and 0.24 g of 2,5-dimethylhexahydro-1H-azepine hydrochloride, and the mixture was stirred for 5 hours at 80° C. The reaction mixture was cooled to near room temperature, a saturated ammonium chloride aqueous solution was added therein, and the mixture was extracted with tert-butyl methyl ether three times. The organic layers were washed with a saturated sodium chloride aqueous solution, dried over anhydrous magnesium sulfate and concentrated. The residue was subjected to silica gel column chromatography to obtain 0.3 g of 1-(6-chloro-5-fluoro pyrimidin-4-yl)-2,5-dimethylhexahydro-1H-azepine.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07732448B2 |
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| 출처 데이터셋 | uspto-grants-2010_06 |
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| ORD ID | ord-2d1e09f46e474b0085885b105c68352b |
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| 출처 메모 | uspto-grants-2010_06 |
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