Iodoethane → 2,2-Diethylmalononitrile
反応式
[C:1](#[N:5])[CH2:2][C:3]#[N:4].[CH2:6](I)[CH3:7].[CH3:9][C:10]([O-])(C)C.[K+]>CCCC[N+](CCCC)(CCCC)CCCC.[Br-]>[CH2:9]([C:2]([CH2:6][CH3:7])([C:1]#[N:5])[C:3]#[N:4])[CH3:10]参加物
5
実験手順
Malononitrile (15.2 g) was mixed with TBAB (3.0 g, 4 mol %) and ethyl iodide (36.8 mL, 2 equiv.). After stirring for 30 minutes at room temperature, the mixture was cooled in an ice bath, KOtBu (51.6 g, 2 equiv.) was added portionwise, the ice bath was removed, and the mixture was stirred for 30 minutes at room temperature. Extraction with DCM/H2O, drying over Na2SO4 and evaporation under reduced pressure gave 40 grams of crude material, which was purified by flash chromatography eluting with DCM. This yielded 20.4 grams of an orange oil which solidified upon standing. 1H NMR (400 MHz, CDCl3) δ 1.29 (t, J=7.5 Hz, 6H), 2.00 (q, J=7.5 Hz, 4H).
後処理
- temperaturethe mixture was cooled in an ice bath
- customthe ice bath was removed
- stirringthe mixture was stirred for 30 minutes at room temperature
- extractionExtraction with DCM/H2O
- dry with materialdrying over Na2SO4 and evaporation under reduced pressure
出典と根拠
- ORDレコード
- ord-70c666ce7b4a4ede94971688eaf95325
- 出典データセット
- uspto-grants-2010_06
- 特許番号
- US07728018B2
反応ノート
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