참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Methyl iodide | HCID 6328 | — |
| 반응물 | Carbon Disulfide | HCID 6348 | — |
| 반응물 | Chloroacetonitrile | HCID 7856 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | Acetylacetone | HCID 31261 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 4-Acetyl-3-methyl-5-(methylthio)thiophene-2-carbonitrile | HCID 2820186 | — |
반응 단계
To a slurry of 2,4-pentanedione (20 mmol) and K2CO3 (3 equivalents, 60 mmol) in DMF (10 mL) was added CS2 (1.2 equivalents, 24 mmol) and the resulting mixture stirred for 10 minutes. The mixture was cooled to 0° C. then chloroacetonitrile (1.0 equivalent, 20 mmol) was added and the reaction stirred 1 hour then warmed to room temperature and stirred for an additional 2 hours. The reaction mixture was again cooled to 0° C. and methyl iodide (1.05 equivalents, 22 mmol) was added slowly. The resulting mixture was warmed to room temperature. After 12 hours, water was added and the resulting suspension was stirred overnight. The desired product was isolated by filtration after washing with water.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07084159B2 |
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| 출처 데이터셋 | uspto-grants-2006_08 |
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| ORD ID | ord-fab1cf601eeb4f96bf3c58d1ce626549 |
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| 출처 메모 | uspto-grants-2006_08 |
|---|