Malononitrile → 2,2-Bis-(2,2,2-trifluoro-ethyl)-malononitrile
反応式
[C:1](#[N:5])[CH2:2][C:3]#[N:4].IC[CH2:8][C:9]([F:12])([F:11])[F:10].[H-].[Na+]>C1COCC1>[F:10][C:9]([F:12])([F:11])[CH2:8][C:2]([CH2:8][C:9]([F:12])([F:11])[F:10])([C:1]#[N:5])[C:3]#[N:4]参加物
5
実験手順
Malononitril (20.15 mmol) and 1-iodo-3,3,3-trifluoropropane (42.65 mmol) were dissolved in 30 ml dry THF, and the mixture was cooled with an ice/salt bath. 1.61 g NaH (40.3 mmol) was added portionwise, keeping the temperature below 5° C. The reaction mixture was stirred at room temperature for 2 hours and evaporated under reduced pressure. The crude material was purified by flash chromatography eluting with DCM, yielding 0.76 grams of an oil. 1H NMR (400 MHz, CDCl3) δ 2.62-2.49 (m, 4H), 2.31-2.24 (m, 4H)
後処理
- temperaturethe mixture was cooled with an ice/salt bath
- customthe temperature below 5° C
- customevaporated under reduced pressure
- customThe crude material was purified by flash chromatography
- washeluting with DCM
出典と根拠
- ORDレコード
- ord-a23d62bb03b44b8aa4bbb58712329041
- 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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