関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | Methyl bromoacetate | HCID 60984 | — |
| 反応物 | N-(4-Chlorophenyl)-3-methoxy-benzenesulfonamide | HCID 57788151 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | [(4-Chlorophenyl)-(3-methoxy-benzenesulphonyl)-amino]-acetic acid methyl ester | HCID 57788185 | — |
反応手順
To a solution of N-(4-chlorophenyl)-3-methoxy-benzenesulfonamide (900 mg, 3.02 mmol) in anhydrous THF (40 mL) was added sodium hydride (146 mg, 3.62 mmol) at 0-5° C. under nitrogen. The mixture was stirred at 25° C. for 30 minutes. Methyl bromoacetate (463 mg, 3.02 mmol) was then added, stirred for 1 h at 25° C. A further amount of methyl bromoacetate (232 mg, 1.51 mmol) was added, and stirring continued for another 12 h. The reaction mixture was quenched with saturated aqueous ammonium chloride solution, and extracted with ethyl acetate (3×20 ml). The combined organic layer was washed with water, dried (Na2SO4), evaporated under reduced pressure to yield the title compound as oily compound, which was used as such in the next step. Yield: 1.03 g (92%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07932269B2 |
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| 出典データセット | uspto-grants-2011_04 |
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| ORD ID | ord-97bbd1237ad14f33a5318303ad7f683c |
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| 出典メモ | uspto-grants-2011_04 |
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