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Dimethyl Sulfate → 5-Bromo-3-methyl-2-(methylthio)pyrimidin-4(3H)-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethyl Sulfate | HCID 6497 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | 5-Bromo-2-(methylsulfanyl)pyrimidin-4(3H)-one | HCID 240565 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 5-Bromo-3-methyl-2-(methylthio)pyrimidin-4(3H)-one | HCID 3264666 | 94.5% |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07897607B2 |
| 出典データセット | uspto-grants-2011_03 |
| ORD ID | ord-d4e65b5a47f349258865a7eb68080063 |
| 出典メモ | uspto-grants-2011_03 |