関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethyl Sulfoxide | HCID 679 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 1-Chloro-2-fluoro-4-methoxy-5-nitrobenzene | HCID 53403289 | — |
| 反応物 | 1-[2-(Methylsulfonyl)ethyl]piperazine hydrochloride | HCID 66649667 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1-[2-Chloro-5-(methyloxy)-4-nitrophenyl]-4-[2-(methylsulfonyl)ethyl]piperazine | HCID 59452634 | 91.3% |
反応手順
To 1-chloro-2-fluoro-4-(methyloxy)-5-nitrobenzene (Example 104, Step B) (0.822 g, 4.0 mmol), 4-[2-(methylsulfonyl)ethyl]piperazine hydrochloride (Example 148, Step B) (0.915 g, 4.0 mmol), and K2CO3 (1.7 g, 12 mmol) was added DMSO (8 mL). The reaction was heated to 100° C. for two days. The reaction was determined to be complete by TLC. The reaction mixture was diluted with H2O and extracted with DCM and EtOAc sequentially for two iterations. The organic was dried (MgSO4), filtered, and rotovapped down. Purification by flash chromatography provided the title compound of Step A (1.38 g, 91%). MS (M+H, ES+) 378.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08093239B2 |
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| 出典データセット | uspto-grants-2012_01 |
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| ORD ID | ord-86d4005b11134c4792f37dc014c8d999 |
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| 出典メモ | uspto-grants-2012_01 |
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