関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Bromine | HCID 24408 | — |
| 反応物 | (4-Methoxy-phenyl)thiazol-2-yl-amine | HCID 956680 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | (5-Bromo-thiazol-2-yl)-(4-methoxy-phenyl)-amine | HCID 12348632 | — |
反応手順
A 1 M solution of Br2 in DMF (12.9 mL, 13.2 mmol) is added dropwise to a solution of (4-methoxy-phenyl)-thiazol-2-yl-amine (2.72 g, 13.2 mmol) in DMF (40 mL), under an argon atmosphere. During the addition, the internal temperature of the reaction mixture is kept below 26° C. The mixture is stirred for 20 min at 25° C. and concentrated in vacuo. Purification of the crude product by silica gel (250 g) column chromatography (CH2Cl2/MeOH, 99/1) affords the title compound: ES-MS: 287.0 [M+H]+; single peak at tR=7.99 min (System 1); Rf=0.47 (CH2Cl2/MeOH, 98/2).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07795288B2 |
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| 出典データセット | uspto-grants-2010_09 |
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| ORD ID | ord-780cd8bd1e934ef988ac08edce26a815 |
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| 出典メモ | uspto-grants-2010_09 |
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