関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1,1'-Thiocarbonyldiimidazole | HCID 80264 | — |
| 反応物 | 4-[4-(Sec-butyl)-1-piperazinyl]benzenamine | HCID 21958917 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1-(4-Isothiocyanatophenyl)-4-(sec-butyl)piperazine | HCID 9856828 | 87.1% |
反応手順
A solution of 4-[4-(sec-butyl)-1-piperazinyl]benzenamine (3.5 g, 15 mmol) (from Step B above) in N,N-dimethylformamide (40 mL) was added dropwise over 20 min to a cooled (−15° C.) solution of thiocarbonyldiimidazole (2.68 g, 15.03 mmol) (Aldrich) in N,N-dimethylformamide (15 mL). After the addition was complete, the mixture was stirred at −15° C. for 20 min, then the cooling bath was removed and the solution was stirred for 1 h. Ice-water (800 ml) was added and the mixture was stirred for 30 min. The solid was filtered off and washed with water and dried under vacuum to give 1-(4-isothiocyanatophenyl)-4-(sec-butyl)piperazine (3.6 g, 87%) as a purple solid.
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-0384dff13c2340f491f72741cfa3d6a8 |
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| 出典メモ | uspto-grants-2006_08 |
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