関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetonitrile | HCID 6342 | — |
| 反応物 | p-Chlorophenacyl bromide | HCID 68303 | — |
| 生成物 | 2-Amino-1-(4-chlorophenyl)ethan-1-one hydrochloride | HCID 2798211 | 50% |
反応手順
A mixture of 2-bromo-1-(4-chlorophenyl)ethanone (1.0 eq.) and NaN(CHO)2 (1.1 eq.) in acetonitrile (1.5 mL per mmol) was heated to reflux for 4 h at 105° C. ext. temperature. The formed sodium bromide was removed by filtration and the filtrate concentrated in vacuo. The residue was dissolved in ethanol (2.5 mL per mmol) and conc. aq. hydrochloric acid (0.9 mL per mmol) added at ambient temperature. After stirring for 72 h at room temperature the solids were filtered off and washed with ethanol (1×0.5 mL per mmol). Drying of the solids afforded 2-amino-1-(4-chlorophenyl)ethanone hydrochloride in ca. 50% yield that was used in the next step without purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08017555B2 |
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| 出典データセット | uspto-grants-2011_09 |
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| ORD ID | ord-964b167cc6c84c37b09f3b27399e11ba |
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| 出典メモ | uspto-grants-2011_09 |
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