関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Bromine | HCID 24408 | — |
| 反応物 | N-(2,3-dihydro-1,4-benzodioxin-5-yl)acetamide | HCID 658593 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | N-(8-Bromobenzo[1,4]dioxan-5-yl)-acetamide | HCID 23269228 | 86.8% |
反応手順
To a solution of compound 8C (0.80 g, 4.15 mmol) in chloroform (2.4 mL) cooled to −20° C. was slowly added a solution of bromine (0.22 mL, 4.35 mmol) in chloroform (1 mL) so that the reaction temperature was maintained below −10° C. The reaction was stirred at 0° C. for 5 min, and then quenched immediately with water. The mixture was extracted with CH2Cl2 (3×), the combined extracts washed with saturated NaHCO3, brine, dried (Na2SO4), filtered and concentrated under reduced pressure. The residue was chromatographed (silica gel) eluting with CH2Cl2 to afford the title compound (0.98 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07405234B2 |
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| 出典データセット | uspto-grants-2008_07 |
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| ORD ID | ord-a0270390e7904d468a99460862bd2505 |
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| 出典メモ | uspto-grants-2008_07 |
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