関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methyl Isocyanate | HCID 12228 | — |
| 反応物 | (R)-4-bromo-alpha-methylbenzylamine | HCID 853000 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1-[1-(4-Bromo-phenyl)ethyl]-3-methyl-urea | HCID 47127327 | 94% |
反応手順
To a stirred solution of (R)-(+)-1-(4-bromophenyl)ethylamine (0.5 g, 2.49 mmol) in anhydrous CH2Cl2 was added methyl isocyanate (0.15 mL, 2.49 mmol). The resulting solution was stirred at 25° C. overnight. CH2Cl2 was evaporate and residue partitioned between EtOAC and 1 N HCl. The organic layer was washed with H2O, brine and dried over Na2SO4. The solvent was removed in vacuo and the residue was purified by flash column chromatography (80% EtOAc in hexanes) to provide the desired product (0.60 g, 94%) as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07148226B2 |
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| 出典データセット | uspto-grants-2006_12 |
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| ORD ID | ord-2ab5911dda914485bf2df388fee5d0f1 |
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| 出典メモ | uspto-grants-2006_12 |
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