Malononitrile → 2,2-Bis-(2,2,2-trifluoro-ethyl)-malononitrile

HRID 1024370

反応式

HRID 1024370 の反応式
[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

反応物 3

HCID 8010MalononitrileHCID 24758Sodium hydrideHCID 1561651,1,1-Trifluoro-3-iodopropane

生成物 1

HCID 866254102,2-Bis-(2,2,2-trifluoro-ethyl)-malononitrile収率 16.4%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

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

  1. temperaturethe mixture was cooled with an ice/salt bath
  2. customthe temperature below 5° C
  3. customevaporated under reduced pressure
  4. customThe crude material was purified by flash chromatography
  5. washeluting with DCM

出典と根拠

ORDレコード
ord-cbc0d984f3a944c9a7df439d4f780def
出典データセット
uspto-grants-2014_05
特許番号
US08722887B2

関連ノート

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