関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Formamidine acetate | HCID 160693 | — |
| 反応物 | Sodium Methoxide | HCID 10942334 | — |
| 反応物 | 4-Ethoxymethylene-2,6-dimethyl-3,5-heptanedione | HCID 22648765 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 5-Isopropylcarbonyl-4-isopropylpyrimidine | HCID 13147451 | 89% |
反応手順
11.5 g (60 mmol) of a 28% sodium methoxide solution was dissolved in 100 ml of methanol, and 5.6 g (54 mmol) of formamidine acetate was added, followed by stirring at room temperature for 15 minutes. Then, 11.5 g (54 mmol) of 4-ethoxymethylene-2,6-dimethyl-3,5-heptanedione was added under cooling with ice. The reaction mixture was further reacted at 50° C. for one hour. The solvent was distilled off under reduced pressure, and 200 ml of water was added, followed by extraction with ethyl acetate. The obtained organic layer was washed with water and then dried over anhydrous magnesium sulfate. Ethyl acetate was distilled off under reduced pressure, and the residue was purified by silica gel column chromatography (developing solvent/n-hexane:ethyl acetate=4:1) to obtain 9.2 g (yield: 89%) of 5-isopropylcarbonyl-4-isopropylpyrimidine as slightly yellow liquid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06806230B1 |
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| 出典データセット | uspto-grants-2004_10 |
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| ORD ID | ord-be52784d279843dcac2df280eb90819f |
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| 出典メモ | uspto-grants-2004_10 |
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