Acetonitrile → 3-Cyclohexyl-3-oxopropanenitrile
反応式
[CH3:1][C:2]#[N:3].[Li]N([Si](C)(C)C)[Si](C)(C)C.[CH:14]1([C:20](OC)=[O:21])[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]1>C1COCC1>[CH:14]1([C:20](=[O:21])[CH2:1][C:2]#[N:3])[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]1参加物
5
実験手順
A solution of 0.53 mL (10 mmol) of MeCN in 5 ml of THF was cooled in −78° C. bath and 12 mL of 1M LiN(TMS)2 was added. After 5 min, 0.75 mL (5.2 mmol) of methyl cyclohexane carboxylate was added. The cold bath was removed after 1 hr and stirring was continued for another 1 hr. The reaction was acidified with 1.2 N HCl and extracted with ether. The ether layer was washed with brine, dried and concentrated. The residue was chromatographed using a gradient of 10-50% EtOAc-hexane to furnish the desired product.
後処理
- customThe cold bath was removed after 1 hr
- waitwas continued for another 1 hr
- extractionextracted with ether
- washThe ether layer was washed with brine
- customdried
- concentrationconcentrated
- customThe residue was chromatographed
出典と根拠
- ORDレコード
- ord-0fd634d9f9dd4fc187e65e5ee4606e2b
- 出典データセット
- uspto-grants-2008_06
- 特許番号
- US07390835B2
反応ノート
読み込み中…