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Water → 2,4-Dichloro-6-(4,5-dihydro-1H-imidazol-2-yl)benzenamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Ethylenediamine | HCID 3301 | — |
| 反応物 | 2,4-Dichloro-6-(trifluoromethyl)aniline | HCID 1268255 | — |
| 反応物 | Butyllithium | HCID 178418339 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | 2,4-Dichloro-6-(4,5-dihydro-1H-imidazol-2-yl)benzenamine | HCID 11817072 | 36.2% |
反応手順
To a solution of ethylene diamine (1.2 mL, 18 mmol) in ethyl ether (50 mL) at −20° C. was added n-butyl lithium (6.4 mL, 2.5 M in hexanes, 16 mmol). The mixture was stirred at 0° C. for 0.3 hour before the addition of 2,4-dichloro-6-trifluoromethyl aniline (0.92 g, 4.2 mmol). The mixture was stirred at 0° C. for an additional 1.5 hours, at which point water (0.36 mL, 20 mmol) was added and the solvent was removed under reduced pressure. Purification by flash column chromatography (silica gel, 1% to 10% methanol in dichloromethane) to give the title compound of Step A (0.35 g) as a yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07326704B2 |
| 出典データセット | uspto-grants-2008_02 |
| ORD ID | ord-108abbfac5ef4efa9ff9a1344a16d7e8 |
| 出典メモ | uspto-grants-2008_02 |