Dimethylformamide → 5-Hexylthiophene-2-carboxaldehyde

HRID 425248

반응식

HRID 425248 반응식
C([Li])CCC.[CH2:6]1[CH2:10][O:9][CH2:8][CH2:7]1.[CH2:11]([C:17]1[S:18]C=CC=1)[CH2:12][CH2:13][CH2:14][CH2:15][CH3:16].CN(C=O)C>[Cl-].[NH4+]>[CH2:11]([C:17]1[S:18][C:6]([CH:10]=[O:9])=[CH:7][CH:8]=1)[CH2:12][CH2:13][CH2:14][CH2:15][CH3:16]

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 8028TetrahydrofuranHCID 877932-HexylthiopheneHCID 178418339Butyllithium

생성물 1

HCID 114696515-Hexylthiophene-2-carboxaldehyde

시약·촉매·용매 1

HCID 25517Ammonium Chloride용매

실험 절차

Under a nitrogen atmosphere at 0° C., 24 ml of n-butyllithium (1.6M in hexane) were added by dripping to a THF solution containing 2-hexylthiophene (5 g). The solution was then stirred for another 15 minutes and, after adding DMF (5 ml), set to room temperature. The resulting solution was then poured into a IN ammonium chloride solution and extracted with methylene chloride. An organic layer was washed with water and dried with anhydrous magnesium sulfate. A crude product was collected by removing the solvent and then purified by a column chromatograph (carrier: silicon dioxide; eluate: hexane/methylene chloride-4/1 (volume ratio)) to obtain 4.6 g of a product.

후처리

  1. customset to room temperature
  2. extractionextracted with methylene chloride
  3. washAn organic layer was washed with water
  4. dry with materialdried with anhydrous magnesium sulfate
  5. customA crude product was collected
  6. customby removing the solvent
  7. custompurified by a column chromatograph (carrier: silicon dioxide; eluate: hexane/methylene chloride-4/1 (volume ratio))

출처 및 근거

ORD 기록
ord-f9a17fe1eb6143a68959b58f958d2121
출처 데이터셋
uspto-grants-2012_01
특허 번호
US08106198B2

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