Hydrochloric Acid → (4-(Trifluoromethyl)benzyl)malononitrile

HRID 1743619

反応式

HRID 1743619 の反応式
[F:1][C:2]([F:16])([F:15])[C:3]1[CH:14]=[CH:13][C:6]([CH:7]=[C:8]([C:11]#[N:12])[C:9]#[N:10])=[CH:5][CH:4]=1.[BH4-].[Na+].Cl>C(O)C>[F:1][C:2]([F:15])([F:16])[C:3]1[CH:4]=[CH:5][C:6]([CH2:7][CH:8]([C:11]#[N:12])[C:9]#[N:10])=[CH:13][CH:14]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 714296(4-(Trifluoromethyl)benzylidene)malononitrileHCID 4311764Sodium borohydride

生成物 1

HCID 10656743(4-(Trifluoromethyl)benzyl)malononitrile収率 51.3%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

First, 4.44 g of (4-(trifluoromethyl)benzylidene)malononitrile was dissolved in 20 ml of ethanol, and while stirring at room temperature, a suspension of 0.19 g of sodium borohydride in 5 ml of ethanol was added dropwise, followed by stirring at room temperature for 30 minutes. Then, 10% hydrochloride acid was added to the reaction mixture, which became acidic and was extracted with diethyl ether. The organic layer was successively washed with 10% hydrochloric acid, a saturated aqueous sodium chloride solution, dried over anhydrous magnesium sulfate, and then concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to give 2.30 g of (4-(trifluoromethyl)benzyl)malononitrile (the intermediate (4)).

後処理

  1. additionwas added dropwise
  2. stirringby stirring at room temperature for 30 minutes
  3. extractionwas extracted with diethyl ether
  4. washThe organic layer was successively washed with 10% hydrochloric acid
  5. dry with materiala saturated aqueous sodium chloride solution, dried over anhydrous magnesium sulfate
  6. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-a93682a602b540c6aedcf7a42b38f024
出典データセット
uspto-grants-2006_03
特許番号
US07011838B2

関連ノート

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