関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Diisopropylamine | HCID 7912 | — |
| 反応物 | 2-Methylpyrazine | HCID 7976 | — |
| 反応物 | Propanoic acid, 2-(4-cyanophenoxy)-2-methyl-, ethyl ester | HCID 205808 | — |
| 反応物 | Butyllithium | HCID 178418339 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Hexane | HCID 8058 | — |
| 生成物 | 4-[1,1-Dimethyl-2-oxo-3-(2-pyrazinyl)propoxy]benzonitrile | HCID 19895605 | 48.8% |
反応手順
10 ml of a 1.2M solution of butyllithium in n-hexane were added to a solution of 1.68 ml of diisopropylamine in 10 ml of tetrahydrofuran while stirring at -78° C. under a nitrogen atmosphere. The solution was stirred for a further 15 minutes and then 0.94 g of 2-methylpyrazine in 20 ml of tetrahydrofuran was added. The solution was allowed to warm to 20° C. and was stirred for 1 hour. The solution was then cooled to -78° C., 2.33 g of ethyl 2-(4-cyanophenoxy)-2-methylpropionate in 30 ml of tetrahydrofuran were added and the mixture was allowed to warm to 20° C. The mixture was treated with 20 ml of water and the solvent was removed by evaporation. The residue was chromatographed on silica gel using ethyl acetate for the elution to give 1.37 g of 4-[1,1-dimethyl-2-oxo-3-(2-pyrazinyl)propoxy]benzonitrile.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04971982 |
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| 出典データセット | uspto-grants-1990_11 |
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| ORD ID | ord-e0f5e1257ee74956bea6c01036f91f65 |
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| 出典メモ | uspto-grants-1990_11 |
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