Hydrochloric Acid → 2-(2,2,3,3,4,4,5,5-Octafluoropentyl)-2-(3,3,4,4,4-pentafluorobutyl)malononitrile

HRID 1443568

反応式

HRID 1443568 の反応式
[F:1][C:2]([F:18])([C:9]([F:17])([F:16])[C:10]([F:15])([F:14])[CH:11]([F:13])[F:12])[CH2:3][CH:4]([C:7]#[N:8])[C:5]#[N:6].I[CH2:20][CH2:21][C:22]([F:28])([F:27])[C:23]([F:26])([F:25])[F:24].C(=O)([O-])[O-].[K+].[K+].Cl>CS(C)=O>[F:1][C:2]([F:18])([C:9]([F:16])([F:17])[C:10]([F:14])([F:15])[CH:11]([F:13])[F:12])[CH2:3][C:4]([CH2:20][CH2:21][C:22]([F:28])([F:27])[C:23]([F:26])([F:25])[F:24])([C:7]#[N:8])[C:5]#[N:6]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 1100921,1,1,2,2-Pentafluoro-4-iodobutaneHCID 25242027(2,2,3,3,4,4,5,5-Octafluoropentyl)propanedinitrile

生成物 1

HCID 247446292-(2,2,3,3,4,4,5,5-Octafluoropentyl)-2-(3,3,4,4,4-pentafluorobutyl)malononitrile収率 21.1%

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

実験手順

1.4 g of 2-(2,2,3,3,4,4,5,5-octafluoropentyl)malononitrile and 1.4 g of 1-iodo-3,3,4,4,4-pentafluorobutane were dissolved in 5 ml of dimethyl sulfoxide, 0.83 g of potassium carbonate was added, and the mixture was stirred at room temperature for 7 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 0.45 g of 2-(2,2,3,3,4,4,5,5-octafluoropentyl)-2-(3,3,4,4,4-pentafluorobutyl)malononitrile (hereinafter, referred to as the present compound (68)).

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-75c58c1092dc4dc88f8b77b557dea6c4
出典データセット
uspto-grants-2010_02
特許番号
US07662402B2

関連ノート

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