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2-Methyl-2-thiopseudourea sulfate → 2-(Methylsulfanyl)-4-[4-(methylsulfanyl)phenyl]-6-(trifluoromethyl)pyrimidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Methyl-2-thiopseudourea sulfate | HCID 75270 | — |
| 反応物 | Sodium Acetate | HCID 517045 | — |
| 反応物 | 1,3-Butanedione, 4,4,4-trifluoro-1-[4-(methylthio)phenyl]- | HCID 10730170 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 2-(Methylsulfanyl)-4-[4-(methylsulfanyl)phenyl]-6-(trifluoromethyl)pyrimidine | HCID 22018314 | 96.2% |
反応手順
To a mixture of 4,4,4-trifluoro-1-[4-(methylthio)phenyl]butane-1,3-dione (5 g) and 2-methyl-2-thiopseudourea sulfate (5.1 g, 0.98 eq) in acetic acid (100 ml) was added sodium acetate (3 g, 2 eq) and heated under reflux for 8 h. The mixture was concentrated in vacuo and water (100 ml) added to give a solid, which was isolated by filtration to give the title compound as a yellow solid (5.8 g, quantitative).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07084148B2 |
| 出典データセット | uspto-grants-2006_08 |
| ORD ID | ord-e51691821d1c445ea36ecbddd8c1bb23 |
| 出典メモ | uspto-grants-2006_08 |