Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Methyl iodide → 6-Iodo-1-(2-methoxyethyl)-2-(methylthio)pyrimidin-4(1H)-one
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Methyl iodide | HCID 6328 | — |
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 반응물 | 6-iodo-1-(2-methoxyethyl)-2-thioxo-2,3-dihydropyrimidin-4(1H)-one | HCID 86684687 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 생성물 | 6-Iodo-1-(2-methoxyethyl)-2-(methylthio)pyrimidin-4(1H)-one | HCID 86684686 | 43.1% |
반응 단계
To a stirring solution of 6-iodo-1-(2-methoxyethyl)-2-thioxo-2,3-dihydropyrimidin-4(1H)-one (9.00 g, 28.83 mmol) in MeCN (200 mL) was added diisopropylethylamine (5.0 mL, 28.83 mmol) and iodomethane (9.0 mL, 144.17 mmol). The reaction mixture was stirred at room temperature for 18 hours, and concentrated in vacuo. The residue was partitioned portioned between CH2Cl2 (200 mL) and 1N aqueous HCl (100 mL). The layers were separated and the organic layer was washed with brine (100 mL), dried over MgSO4 and concentrated in vacuo. The resulting residue was purified by hot trituration with CH2Cl2/heptane to give the title compound (4.05 g, 43%) as a cream colored solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08835449B2 |
| 출처 데이터셋 | uspto-grants-2014_09 |
| ORD ID | ord-abf0a0af5eea47288956e89f8d644661 |
| 출처 메모 | uspto-grants-2014_09 |