Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Methyl iodide → Thiophene-3-carbonitrile, 5-acetyl-4-(4-chlorophenyl)-2-methylthio-
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Methyl iodide | HCID 6328 | — |
| 반응물 | Carbon Disulfide | HCID 6348 | — |
| 반응물 | Chloroacetone | HCID 6571 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 4-Chlorobenzoylacetonitrile | HCID 138308 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | Thiophene-3-carbonitrile, 5-acetyl-4-(4-chlorophenyl)-2-methylthio- | HCID 627943 | — |
반응 단계
3-(4-Chloro-phenyl)-3-oxo-propionitrile (5 mmol) was added to a suspension of K2CO3 (3 equivalents, 15 mmol) in DMF (4.5 mL) and allowed to stir at room temperature. After 10 minutes, CS2 (1.25 equivalents, 7.5 mmol) was added in one portion and the resulting mixture stirred at room temperature for an additional 10 minutes then a solution of 1-chloro-propan-2-one (1.0 equivalent, 5 mmol) in DMF (5 mL) was added. After 1 hour, a solution of MeI (1.1 equivalents, 5.5 mmol) in DMF (2 mL) was added in a dropwise fashion then, after 30 minutes, the mixture was poured onto water and the resulting mixture was stirred vigorously for 12–16 hours to afford a suspension of the desired product. The crude product was isolated by filtration.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07084159B2 |
| 출처 데이터셋 | uspto-grants-2006_08 |
| ORD ID | ord-a8501356412b4821bc14f268d1131b78 |
| 출처 메모 | uspto-grants-2006_08 |