関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethyl Sulfate | HCID 6497 | — |
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | 6-Bromo-3-hydroxy-3-methylindolin-2-one | HCID 66580258 | — |
| 溶媒 | acetonitrile N,N-dimethylformamide | HCID 21891449 | — |
| 生成物 | 6-Bromo-3-methoxy-1,3-dimethylindolin-2-one | HCID 89471914 | — |
反応手順
A solution of 6-bromo-3-hydroxy-3-methylindolin-2-one 7.45 (200 mg, 0.826 mmol) in ACN/DMF (2:1, 6 mL) was cooled to 0° C. Cesium carbonate (942 mg, 2.89 mmol) and dimethyl sulfate (274 μL, 2.89 mmol) were added. The reaction was stirred at 0° C. for 90 min then at room temperature for 4 hours. The mixture was filtered over celite, concentrated and the residue was purified by flash column chromatography on silica gel to afford 6-bromo-3-methoxy-1,3-dimethylindolin-2-one 7.46. 1H NMR (400 MHz, DMSO-d6) δ 7.39-7.25 (m, 3H), 3.14 (s, 3H), 2.85 (s, 3H), 1.40 (s, 3H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09376441B2 |
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| 出典データセット | uspto-grants-2016_06 |
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| ORD ID | ord-5a5b7068e3c449e6961fb87c97327213 |
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| 出典メモ | uspto-grants-2016_06 |
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