関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methyl iodide | HCID 6328 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Ethyl 3,4-dihydro-2H-1,4-benzoxazine-2-carboxylate | HCID 31090 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | ethyl 4-methyl-3,4-dihydro-2H-1,4-benzoxazine-2-carboxylate | HCID 10608998 | 65.5% |
反応手順
In a sealable vessel, potassium carbonate (56 mg, 0.41 mmol) was added to a solution of (±)-ethyl 3,4-dihydro-2H-benzo[b][1,4]oxazine-2-carboxylate (60 mg, 0.29 mmol) and iodomethane (22 □L, 0.35 mmol) in acetone (2 mL). The vessel was sealed and the reaction mixture was stirred at 60° C. for 24 h. The mixture was cooled to ambient temperature, diluted with dichloromethane (60 mL), and the organic layer was extracted with water (10 mL) and half-saturated brine (10 mL). The organic layer was dried over sodium sulfate and concentrated. Purification of the concentrate by flash column chromatography (5% to 10% EtOAc/hexane) afforded the title compound (43 mg, 0.19 mmol). MS m/z: 222 (M+1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07872009B2 |
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| 出典データセット | uspto-grants-2011_01 |
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| ORD ID | ord-ce2e6b8bdf6e4afc9cc84d2f7229f786 |
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| 出典メモ | uspto-grants-2011_01 |
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