関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1,3,5-Trimethyl-1,3,5-triazacyclohexane | HCID 7952 | — |
| 反応物 | Rac-4-cyclohexyl-4-nitro-butyric acid methyl ester | HCID 59438496 | — |
| 生成物 | Rac-5-cyclohexyl-1-methyl-5-nitro-piperidin-2-one | HCID 59438407 | 57.4% |
反応手順
To 4.25 g (18.5 mmol) rac-4-cyclohexyl-4-nitro-butyric acid methyl ester were added 4.56 ml (32.5 mmol) 1,3,5-trimethylhexahydro-1,3,5-triazine and the mixture heated to 100° C. for 4 hours. The reaction mixture was cooled to ambient temperature and adsorbed on silica gel which was transferred on top of a silica gel column and purified by flash-chromatography with a gradient of heptane and 10 to 75% ethyl acetate: 2.55 g of title compound were isolated as colourless oil: MS (m/e): 240 (MH+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09067911B2 |
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| 出典データセット | uspto-grants-2015_06 |
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| ORD ID | ord-bb8e62a8a3df4f6bb21e03134e2b40a3 |
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| 出典メモ | uspto-grants-2015_06 |
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