関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 1-(2-Methoxyphenyl)piperazine | HCID 1346 | — |
| 反応物 | (R)-4-methyl-3-pyridin-2-yl[1,2,3]oxathiazolidine-2,2-dioxide | HCID 22863100 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | (R)-1-(2-Methoxyphenyl)-4-[2-(methyl)-2-(2-pyridinylamino)ethyl]piperazine | HCID 25273062 | 79.2% |
反応手順
9.16 grams (46.6 millimoles) of 1-(2-methoxyphenyl)piperazine in one portion was added under argon to a solution of 10 grams (46.6 millimoles) of (R)4-methyl-3-pyridin-2-yl[1,2,3]oxathiazolidine-2,2-dioxide in 200 milliliters of acetonitrile. The mixture became yellow. After 1/2 hour, the reaction mixture was heated to 50° C. for 1 hour and then stirred at room temperature overnight. Then dilute hydrochloric acid was added. The mixture was washed with ethyl acetate, basified to pH 12 and extracted twice with ethyl acetate. The organic phases were washed with brine, dried (Mg SO4) and subjected to evaporation to give 12.053 grams of the title compound which was purified by columning in the system ethyl ether/hexane (1:1) Al2O3 to afford 9.96 grams of the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06133449 |
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| 出典データセット | uspto-grants-2000_10 |
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| ORD ID | ord-bf48194621b4497cb5ef0f1b6835417f |
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| 出典メモ | uspto-grants-2000_10 |
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