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Methanol → 9-Chloro-3-methyl-5-piperidin-3-yl-5H-isoxazolo[4,3-c]quinolin-4-one hydroiodide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Diethyl Ether | HCID 3283 | — |
| 反応物 | Trimethylsilyl iodide | HCID 85247 | — |
| 反応物 | 3-(9-chloro-3-methyl-4-oxo-5H-isoxazolo[4,3-c]quinolin-5-yl)-piperidine-1-carboxylic acid methyl ester | HCID 9951561 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 9-Chloro-3-methyl-5-piperidin-3-yl-5H-isoxazolo[4,3-c]quinolin-4-one hydroiodide | HCID 21963712 | 97% |
反応手順
Add iodotrimethylsilane (1.87 mL, 13.16 mmol) to a solution of 3-(9-chloro-3-methyl-4-oxo-5H-isoxazolo[4,3-c]quinolin-5-yl)-piperidine-1-carboxylic acid methyl ester (2.06 g, 5.48 mmol) in dichloromethane (40 mL). Stir the solution at room temperature under nitrogen overnight. Add methanol (3.2 mL, 78.93 mmol) dropwise, and stir the reaction at room temperature for 30 minutes. Concentrate the reaction, add to diethyl ether, sonicate, and filtere. Dry the solids on a vacuum pump to give 2.36 g of the title compound as a tan solid, 97% yield. 1H NMR: consistent with structure. MS (ion spray) 318 (M+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07101891B2 |
| 出典データセット | uspto-grants-2006_09 |
| ORD ID | ord-769fcdf1cdd8433c89c93ffe0bcf8a88 |
| 出典メモ | uspto-grants-2006_09 |