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-(Propan-2-yl)piperazin-1-yl]aniline | HCID 9161545 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1-(4-Isothiocyanatophenyl)-4-(1-methylethyl)piperazine | HCID 9878386 | 101.3% |
反応手順
A solution of 4-[4-(1-methylethyl)-1-piperazinyl]benzenamine (1.6 g, ˜6.8 mmol) (from Step B above) in N,N-dimethylformamide (25 mL) was added dropwise over 20 min to a cooled (−15° C.) solution of thiocarbonyldiimidazole (1.4 g, 7.7 mmol) (Aldrich) in N,N-dimethylformamide (30 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 was added and the mixture was extracted with ether. The ether layer was dried (MgSO4), filtered, and evaporated to give 1-(4-isothiocyanatophenyl)-4-(1-methylethyl)piperazine (1.8 g, quantitative yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07105670B2 |
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| 出典データセット | uspto-grants-2006_09 |
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| ORD ID | ord-4d90b5672a4a4d96b1e618b00ce87df6 |
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| 出典メモ | uspto-grants-2006_09 |
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