関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1,1'-Thiocarbonyldiimidazole | HCID 80264 | — |
| 反応物 | 1-[4-(4-Aminophenyl)piperazin-1-yl]ethan-1-one | HCID 736269 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1-(Acetyl)-4-(4-isothiocyanatophenyl)piperazine | HCID 21958899 | 84% |
反応手順
A solution of 1-acetyl-4-(4-aminophenyl)piperazine (1.0 g, 4.6 mmol) (from Step B above) in N,N-dimethylformamide (10 mL) was added dropwise to a cooled (−15° C.) solution of thiocarbonyldiimidazole (855 mg, 4.8 mmol) in N,N-dimethylformamide (10 mL). After the addition was complete, the mixture was stirred at −15° C. for 30 min, then the cooling bath was removed and the solution was stirred for 1 h. Ice-water was added and the mixture was extracted with ether (4×50 mL). The combined ether layers were washed with brine, dried (MgSO4), filtered, and evaporated to give 1-(acetyl)-4-(4 isothiocyanatophenyl)piperazine (1.0 g, 84%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07094896B2 |
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| 出典データセット | uspto-grants-2006_08 |
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| ORD ID | ord-791ac1550fd64af8a5667939b1f90372 |
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| 出典メモ | uspto-grants-2006_08 |
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