참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | 3,4-Dichloro-1,2,5-thiadiazole | HCID 79804 | — |
| 반응물 | Piperazine, hexahydrate | HCID 120181 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 용매 | Sodium chloride; water | HCID 57417360 | — |
| 생성물 | 1-(4-Chloro-[1,2,5]thiadiazol-3-yl)piperazine hydrochloride | HCID 21202042 | 89% |
반응 단계
A mixture of 3,4-dichloro-1,2,5-thiadiazole (4.00 g, 25.8 mmol) and piperazine hexahydrate (25.0 g, 130 mmol) in DMF (25 mL) was heated at 70° C. for 20 minutes. After cooling to ambient temperature, the reaction mixture was basified (11 M NaOH) and brine was added. The resulting mixture was extracted with CHCl3 (×3). The combined organic phases were washed twice with brine/water (1:1), dried (MgSO4) and the solvent was evaporated. The resulting oil was purified by column chromatography on silica gel using CHCl3 as eluent to give 2.77 g (52%) of the title compound as a colourless oil which was converted to its hydrochloride salt: mp 231° C. (dec). Anal (C6H9ClN4S.HCl), C calc 29.89, found 30.4. H. N
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07534794B2 |
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| 출처 데이터셋 | uspto-grants-2009_05 |
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| ORD ID | ord-3bec647fc2294116bc60f4351f38de2b |
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| 출처 메모 | uspto-grants-2009_05 |
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