Hydrochloric Acid → HCID 11075305, 화합물

HRID 749597노트

반응식

HRID 749597 반응식
[Cl:1][C:2]1[CH:13]=[CH:12][C:5]([CH:6]=[C:7]([C:10]#[N:11])[C:8]#[N:9])=[CH:4][CH:3]=1.[CH:14]([Mg]Br)([CH3:16])[CH3:15].Cl>O1CCCC1.[Cu]I>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([CH:6]([CH:7]([C:8]#[N:9])[C:10]#[N:11])[CH:14]([CH3:16])[CH3:15])=[CH:12][CH:13]=1

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 158474-ChlorobenzalmalononitrileHCID 178418365HCID 178418365, 화합물

생성물 1

HCID 11075305HCID 11075305, 화합물수율 52%

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매2회HCID 24350Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)용매

실험 절차

First, 1.02 g of (4-chlorobenzylidene)malononitrile was dissolved in 20 ml of tetrahydrofuran, to which a catalytic amount of copper (I) iodide was added, and while stirring under ice cooling, a solution of isopropyl magnesium bromide in tetrahydrofuran (prepared from 0.34 g of magnesium, 10 ml of tetrahydrofuran, and 1.46 ml of isopropyl bromide) was added dropwise, followed by stirring for 30 minutes under ice cooling. Then, 10% hydrochloric acid was added to the reaction mixture, which became acidic and 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 0.66 g of (1-(4-chlorophenyl)-2-methylpropyl)malononitrile (the intermediate (3)).

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-ad0ec5f19fc54c8b9bd10f11159bc849
출처 데이터셋
uspto-grants-2008_07
특허 번호
US07402691B2

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