Hydrochloric Acid → HCID 22235030, 화합물

HRID 1743617노트

반응식

HRID 1743617 반응식
[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

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 2636762-[1-(4-chlorophenyl)ethylidene]malononitrileHCID 178418373HCID 178418373, 화합물

생성물 1

HCID 22235030HCID 22235030, 화합물수율 69%

시약·촉매·용매 2

HCID 3283Diethyl Ether용매2회HCID 24350Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)용매

실험 절차

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)).

후처리

  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

출처 및 근거

ORD 기록
ord-c3be499209254e1ba9384ff5dac8c6c4
출처 데이터셋
uspto-grants-2006_03
특허 번호
US07011838B2

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