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Diisopropylamine → 3-(1-Methylcyclopropyl)-3-oxopropanenitrile

HRID 452964
ノート
印刷プレビュー

反応式

HRID 452964 の反応式
[CH:1]([NH:4]C(C)C)(C)[CH3:2].[Li]CCCC.[CH3:13][C:14]1([C:17]([O:19]C)=O)[CH2:16][CH2:15]1>C1COCC1>[CH3:13][C:14]1([C:17](=[O:19])[CH2:2][C:1]#[N:4])[CH2:16][CH2:15]1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 7912DiisopropylamineHCID 543995Methyl 1-methylcyclopropane-1-carboxylateHCID 178418339Butyllithium

生成物 1

HCID 133930463-(1-Methylcyclopropyl)-3-oxopropanenitrile収率 89%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
-78 °C

実験手順

To a solution of diisopropylamine (7.43 mL, 52.6 mmol) in 60 mL of THF was added n-BuLi (2.5M) (21.03 mL, 52.6 mmol) at −78° C. The reaction was stirred at −78° C. for 30 min, then acetononitrile (2.76 mL, 52.6 mmol) was added at −78° C. and the reaction was stirred for 30 min, then methyl 1-methylcyclopropanecarboxylate (3 g, 52.6 mmol) was added at −78° C. The reaction was stirred at −78° C. for 1 hour and then allowed to warm up at room temperature overnight. The solvent was evaporated and the solid dissolved in water. The aqueous layer was washed with ether and then acidified with 6N HCl to pH 2-3. The aqueous layer was extracted with ether. The organic layer was dried with MgSO4 and concentrated to afford the title compound (2.89 g, 89%). MS (DCI/NH3) m/z 124 (M+H)+.

後処理

  1. additionwas added at −78° C.
  2. stirringthe reaction was stirred for 30 min
  3. stirringThe reaction was stirred at −78° C. for 1 hour
  4. temperatureto warm up at room temperature overnight
  5. customThe solvent was evaporated
  6. dissolutionthe solid dissolved in water
  7. washThe aqueous layer was washed with ether
  8. extractionThe aqueous layer was extracted with ether
  9. dry with materialThe organic layer was dried with MgSO4
  10. concentrationconcentrated

出典と根拠

ORDレコード
ord-baff84edc84347e5a18b166f9ed6785a
出典データセット
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08492371B2

反応ノート

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