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Piperazine → 6-Chloro-2-(piperazin-1-yl)-1,3-benzothiazole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Piperazine | HCID 4837 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2,6-Dichlorobenzothiazole | HCID 77176 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 6-Chloro-2-(piperazin-1-yl)-1,3-benzothiazole | HCID 2746595 | 100% |
反応手順
To a stirred solution of 1.07 g (5.24 mmol) of 2,6-dichlorobenzothiazole in dry DMF (25 mL) was added 2.4 g of potassium carbonate (15.7 mmol) and 0.5 g of piperazine (5.8 mmol). The mixture was stirred at room temperature for 4 h. When the reaction was complete it was partitioned between EtOAc (150 mL) and water (50 mL) and separated. The aqueous layer was extracted with EtOAC (2×100 mL). The combined organic layers were then washed with water (2×25 mL), brine, dried over Na2SO4, and the solvent was removed under reduced pressure to give 1.33 g (100%) of desired product as a white solid. MS (electrospray): exact mass calculated for C11H12ClN3S, 253.04; m/z found, 254.0 [M+H]+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07452890B2 |
| 出典データセット | uspto-grants-2008_11 |
| ORD ID | ord-51159eefe5904fac8116be022d2eccd8 |
| 出典メモ | uspto-grants-2008_11 |