참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | 2,6-Dimethylpiperazine | HCID 66056 | — |
| 반응물 | 3,4-Dichloro-1,2,5-thiadiazole | HCID 79804 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 1-(4-Chloro-[1,2,5]thiadiazol-3-yl)-3,5-dimethyl-piperazine | HCID 59013949 | 97% |
반응 단계
2,6-Dimethyl-piperazine (8.1 g, 71 mmol) was heated to 100° C. in DMF (8.0 ml). 3,4-Dichloro-1,2,5-thiadiazole (3.3 ml, 35 mmol) was added and the mixture stirred at 100° C. for 3-4 h. The reaction mixture was poured into H2O and extracted with EtOAc (4×). The combined EtOAc extractions were washed with sat'd NaHCO3 (1×), sat'd NaCl (1×), dried (Na2SO4), and concentrated in vacuo to give 7.9 g (97%) of 1-(4-chloro-[1,2,5]thiadiazol-3-yl)-3,5-dimethyl-piperazine which was used without further purification. 1H NMR (CDCl3) 3.90-3.86 (m, 2H), 3.05 (m, 2H), 2.52 (m, 2H), 1.12 (d, 6H) ppm. LC-MS (MH+)=233.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08013156B2 |
|---|
| 출처 데이터셋 | uspto-grants-2011_09 |
|---|
| ORD ID | ord-3ea7e018ba6f4de69e625dffc4e04115 |
|---|
| 출처 메모 | uspto-grants-2011_09 |
|---|
