Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Dimethyl Sulfate → 5-Bromo-3-methyl-2-(methylthio)pyrimidin-4(3H)-one
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Dimethyl Sulfate | HCID 6497 | — |
| 반응물 | Potassium Hydroxide | HCID 14797 | — |
| 반응물 | 5-Bromo-2-(methylsulfanyl)pyrimidin-4(3H)-one | HCID 240565 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | 5-Bromo-3-methyl-2-(methylthio)pyrimidin-4(3H)-one | HCID 3264666 | 94.5% |
반응 단계
To a mixture containing 0.70 g (5.5 mmol) of dimethyl sulfate and 0.25 g (4.5 mmol) of potassium hydroxide in 10 ml of tetrahydrofuran was added 0.5 g (2.25 mmol) of 5-Bromo-2-(methylthio)pyrimidin-4(3H)-one in portions over 15 min. After complete addition, the mixture was stirred overnight then diluted with ethyl acetate and washed with water. The organic phase was dried over magnesium sulfate. Filtration, removal of solvent and purification of the residue via Biotage chromatography eluting with 20% ethyl acetate/dichloromethane gave 0.5 g (94%) of product.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07897607B2 |
| 출처 데이터셋 | uspto-grants-2011_03 |
| ORD ID | ord-d4e65b5a47f349258865a7eb68080063 |
| 출처 메모 | uspto-grants-2011_03 |