Hydrochloric Acid → HCID 86612545、化合物

HRID 1443559ノート

反応式

HRID 1443559 の反応式
[C:1](#[N:5])[CH2:2][C:3]#[N:4].I[CH2:7][CH2:8][C:9]([F:18])([C:14]([F:17])([F:16])[F:15])[C:10]([F:13])([F:12])[F:11].C(=O)([O-])[O-].[K+].[K+].Cl>COCCOC>[F:18][C:9]([C:14]([F:17])([F:16])[F:15])([C:10]([F:13])([F:12])[F:11])[CH2:8][CH2:7][C:2]([CH2:7][CH2:8][C:9]([C:10]([F:11])([F:12])[F:13])([F:18])[C:14]([F:17])([F:16])[F:15])([C:1]#[N:5])[C:3]#[N:4]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 8010MalononitrileHCID 11430Potassium CarbonateHCID 6296591,1,1,2-Tetrafluoro-4-iodo-2-(trifluoromethyl)butane

生成物 1

HCID 86612545HCID 86612545、化合物収率 0.9%

試薬・触媒・溶媒 1

HCID 80711,2-Dimethoxyethane溶媒

実験手順

0.66 g of malononitrile and 9.7 g of 1-iodo-3,4,4,4-tetrafluoro-3-trifluoromethylbutane were dissolved in 10 ml of ethylene glycol dimethyl ether, 4.1 g of potassium carbonate was added, and the mixture was stirred at room temperature for 15 hours. Thereafter, dilute hydrochloric acid 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 0.04 g of 2,2-bis(3,4,4,4-tetrafluoro-3-trifluoromethylbutyl)malononitrile (hereinafter, referred to as the present compound (56)).

後処理

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

出典と根拠

ORDレコード
ord-5903ff54f6da4f4ea6eae9fc3099a9d5
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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