Water → 2-(5-Fluoropentyl)-2-(3,3,3-trifluoropropyl)malononitrile

HRID 1443558ノート

反応式

HRID 1443558 の反応式
C(N(S(F)(F)[F:7])CC)C.O[CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][C:16]([CH2:21][CH2:22][C:23]([F:26])([F:25])[F:24])([C:19]#[N:20])[C:17]#[N:18].O>C(Cl)(Cl)Cl>[F:7][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][C:16]([CH2:21][CH2:22][C:23]([F:26])([F:25])[F:24])([C:19]#[N:20])[C:17]#[N:18]

参加物

5

反応物 3

HCID 962WaterHCID 123472(Diethylamino)sulfur trifluorideHCID 588790372-(5-Hydroxypentyl)-2-(3,3,3-trifluoropropyl)malononitrile

生成物 1

HCID 866125442-(5-Fluoropentyl)-2-(3,3,3-trifluoropropyl)malononitrile収率 29.8%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒2 回

実験手順

0.29 g of diethylaminosulfur trifluoride was dissolved in 5 ml of chloroform and thereto was added dropwise at 0° C. 0.40 g of 2-(5-hydroxypentyl)-2-(3,3,3-trifluoropropyl)malononitrile dissolved in 3 ml of chloroform. The mixture was stirred at room temperature for 9 hours. Thereafter, water was added to the reaction mixture, followed by extraction with methyl tert-butyl ether. The organic layer was washed successively with water, aqueous saturated sodium hydrogen carbonate and aqueous saturated sodium chloride, dried over anhydrous magnesium sulfate, and then concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to obtain 0.12 g of 2-(5-fluoropentyl)-2-(3,3,3-trifluoropropyl)malononitrile (hereinafter, referred to as the present compound (55)).

後処理

  1. additionwas added dropwise at 0° C
  2. extractionfollowed by extraction with methyl tert-butyl ether
  3. washThe organic layer was washed successively with water, aqueous saturated sodium hydrogen carbonate and aqueous saturated sodium chloride
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-72167660c5b94f48aa76aacf57b3c998
出典データセット
uspto-grants-2010_02
特許番号
US07662402B2

反応ノート

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