2-(4,6-Dichloropyrimidin-2-yl)acetonitrile → (Pyrimidin-2-yl)acetonitrile
反応式
Cl[C:2]1[CH:7]=[C:6](Cl)[N:5]=[C:4]([CH2:9][C:10]#[N:11])[N:3]=1>CCOC(C)=O.CO.[Pd]>[N:3]1[CH:2]=[CH:7][CH:6]=[N:5][C:4]=1[CH2:9][C:10]#[N:11]参加物
4
実験手順
To a solution of 2-(4,6-dichloropyrimidin-2-yl)acetonitrile (4.10 g, 21.8 mmol) and TEA (6.07 ml, 43.6 mmol) in EtOAc/MeOH (1/1, 80 mL) was added 10% Pd/C (800 mg) and the solution was vigorously stirred for 2.5 h under H2 atmosphere (1 atm). The reaction was filtered through celite and washed the celite with MeOH. The combined filtrates were concentrated under reduced pressure and purified by flash chromatography (SiO2, 40-6% EtOAc/flexanes, gradient elution) to provide 2-(pyrimidin-2-yl)acetonitrile (1.56 g, 13.1 mmol, 60%) as a pale red liquid.
後処理
- filtrationThe reaction was filtered through celite
- washwashed the celite with MeOH
- concentrationThe combined filtrates were concentrated under reduced pressure
- custompurified by flash chromatography (SiO2, 40-6% EtOAc/flexanes, gradient elution)
出典と根拠
- ORDレコード
- ord-a41755a6bec04810bd62305aedce7542
- 出典データセット
- uspto-grants-2014_07
- 特許番号
- US08772296B2
反応ノート
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