Hydrochloric Acid → HCID 22235030、化合物

HRID 1743617ノート

反応式

HRID 1743617 の反応式
[Cl:1][C:2]1[CH:14]=[CH:13][C:5]([C:6](=[C:8]([C:11]#[N:12])[C:9]#[N:10])[CH3:7])=[CH:4][CH:3]=1.[CH3:15][Mg]I.Cl>C(OCC)C.[Cu]I>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([C:6]([CH:8]([C:11]#[N:12])[C:9]#[N:10])([CH3:15])[CH3:7])=[CH:13][CH:14]=1

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 2636762-[1-(4-chlorophenyl)ethylidene]malononitrileHCID 178418373HCID 178418373、化合物

生成物 1

HCID 22235030HCID 22235030、化合物収率 69%

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒2 回HCID 24350Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)溶媒

実験手順

First, 1.00 g of (4-chloro-α-methylbenzylidene)malononitrile of the formula: was dissolved in 20 ml of diethyl ether, to which a catalytic amount of copper (I) iodide was added, and while stirring under ice cooling, a solution of methyl magnesium iodide in diethyl ether (prepared from 0.30 g of magnesium, 10 ml of diethyl ether, and 0.86 ml of methyl iodide) was added dropwise, followed by stirring for 30 minutes under ice cooling. Then, 10% hydrochloric acid was added to the reaction mixture, which was extracted with ethyl 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 0.74 g of (1-(4-chlorophenyl)-1-methylethyl)malononitrile (the intermediate (2)).

後処理

  1. additionwas added
  2. stirringby stirring for 30 minutes under ice cooling
  3. extractionwas extracted with ethyl 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-c3be499209254e1ba9384ff5dac8c6c4
出典データセット
uspto-grants-2006_03
特許番号
US07011838B2

反応ノート

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