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Dimethylformamide dimethyl acetal → 4-Methyl-2-(methylsulfanyl)pyrimidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethylformamide dimethyl acetal | HCID 78373 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 2-Mercapto-4-methylpyrimidine hydrochloride | HCID 178428687 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 4-Methyl-2-(methylsulfanyl)pyrimidine | HCID 821261 | 84.6% |
反応手順
To 2-mercapto-4-methylpyrimidine·HCl (50.0 g, 0.307 mole) in toluene (750 mL), under argon, was added diisopropylethylamine (80.0 mL, 0.461 mole) followed by N,N-dimethylformamide dimethyl acetal (100 mL) and the mixture heated to reflux for 4 hours. Upon cooling, the reaction was concentrated in vacuo to an oil, dissolved in ether (400 mL), and washed with water (2×50 mL). The organic extract was dried over anhydrous sodium sulfate, filtered and concentrated to an oil which was vacuum distilled to give 2-methylthio-4-methylpyrimidine (36.4 g) as an oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05859041 |
| 出典データセット | uspto-grants-1999_01 |
| ORD ID | ord-a19ceaf028184881a3776d4a7655c208 |
| 出典メモ | uspto-grants-1999_01 |