反応式
[H-].[Na+].O1CCCC1.[CH2:8]([C:10]([CH3:17])([CH2:15][CH3:16])[C:11]([O:13]C)=O)[CH3:9].[H-].[C:19](#[N:21])[CH3:20]>C(O)C>[CH2:15]([C:10]([CH3:17])([CH2:8][CH3:9])[C:11]([CH2:20][C:19]#[N:21])=[O:13])[CH3:16]参加物
実験手順
To a suspension of 96 g. of sodium hydride, as a 50% dispersion in mineral oil, in 300 ml. of dry tetrahydrofuran was added, with stirring, 63 g. of acetonitrile and 114 g. of methyl 2-ethyl-2-methylbutyrate. The mixture was then heated gently to 60°-65° and allowed to reflux gently at that temperature overnight. It was then cooled to ice bath temperature, and 2-ml. portions of ethanol were added to decompose the remaining hydride. When the mixture did not foam on further ethanol addition, the mixture was evaporated under vacuum to dryness, and the residue was dumped into 4 liters of water. The aqueous mixture was extracted with hexane to remove the mineral oil, and it was then made acid to pH 2 and was extracted with two 1-liter portions of diethyl ether. The ether was dried over magnesium sulfate and evaporated under vacuum to obtain 122 g. of the desired acetonitrile.
後処理
- additionTo a suspension of 96 g
- temperatureThe mixture was then heated gently to 60°-65°
- temperatureto reflux gently at that temperature overnight
- temperatureIt was then cooled to ice bath temperature, and 2-ml
- customthe mixture was evaporated under vacuum to dryness
- extractionThe aqueous mixture was extracted with hexane
- customto remove the mineral oil, and it
- extractionwas extracted with two 1-liter portions of diethyl ether
- dry with materialThe ether was dried over magnesium sulfate
- customevaporated under vacuum
- customto obtain 122 g
出典と根拠
- ORDレコード
- ord-1c4edb83a7a4493689aab3ae7451f2f1
- 出典データセット
- uspto-grants-1983_10
- 特許番号
- US04411753
関連ノート
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