関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | N-(2-Methoxyethyl)ethylamine | HCID 546877 | — |
| 反応物 | HCID 178485964 | HCID 178485964 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | HCID 178464021 | HCID 178464021 | 83% |
反応手順
A solution of 200 mg (corresponds to 0.43 mmol) of trans-Methanesulfonic acid 3-{4-[(4-chloro-phenoxycarbonyl)-methyl-amino]-cyclohexyl}-prop-2-ynyl ester in 4.3 ml of methanol was cooled to 0° C., treated with 0.44 ml (1 mmol) of Ethyl-(2-methoxy-ethyl)-amine and stirred over night at RT. The solvent was evaporated and the residue extracted with aqueous saturated NaHCO3/Et2O (3×). The organic phase was dried with Na2SO4, filtered and evaporated. Purification by flash column chromatography on silica gel (CH2Cl2/MeOH 99:1) gave 144 mg (83%) of pure trans-(4-{3-[Ethyl-(2-methoxy-ethyl)-amino]-prop-1-ynyl}-cyclohexyl)-methyl-carbamic acid 4-chloro-phenyl ester, MS: 407 (MH+, 1Cl). The following compounds were prepared from the corresponding mesylates and secondary amines:
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06858651B2 |
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| 出典データセット | uspto-grants-2005_02 |
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| ORD ID | ord-edb488e4a25f4f5bb16d32bd7b37e45c |
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| 出典メモ | uspto-grants-2005_02 |
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