Water → HCID 14044829, 화합물

HRID 494917노트

반응식

HRID 494917 반응식
[OH:1][C:2]1[CH:7]=[C:6]([O:8][CH3:9])[CH:5]=[CH:4][C:3]=1[C:10](=[O:12])[CH3:11].C(=O)([O-])[O-].[K+].[K+].[CH2:19](Br)[CH:20]=[CH2:21].O>CN(C)C=O.C(OCC)(=O)C>[CH2:21]([O:1][C:2]1[CH:7]=[C:6]([O:8][CH3:9])[CH:5]=[CH:4][C:3]=1[C:10](=[O:12])[CH3:11])[CH:20]=[CH2:19]

참가 물질

7

반응물 4

HCID 962WaterHCID 7841Allyl bromideHCID 11092PaeonolHCID 11430Potassium Carbonate

생성물 1

HCID 14044829HCID 14044829, 화합물

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

실험 절차

5.00 g of 2′-hydroxy-4′-methoxyacetophenone was dissolved in 40 ml of N,N-dimethylformamide at room temperature. Thereafter, 4.16 g of potassium carbonate and 2.80 ml of allyl bromide were successively added to the reaction solution. After the disappearance of materials had been confirmed, water and ethyl acetate were added to the reaction solution, so as to separate an organic layer. The obtained organic layer was washed with water and a saturated sodium chloride aqueous solution, and then dried over anhydrous magnesium sulfate. After removing the drying agent by filtration, the organic layer was concentrated under a reduced pressure, and the residue was then purified by silica gel column chromatography (hexane/ethyl acetate), so as to obtain 5.60 g of the subject compound.

후처리

  1. customso as to separate an organic layer
  2. washThe obtained organic layer was washed with water
  3. dry with materiala saturated sodium chloride aqueous solution, and then dried over anhydrous magnesium sulfate
  4. customAfter removing the drying agent
  5. filtrationby filtration
  6. concentrationthe organic layer was concentrated under a reduced pressure
  7. customthe residue was then purified by silica gel column chromatography (hexane/ethyl acetate)

출처 및 근거

ORD 기록
ord-f5a47944179a41319aa57db2cd9ce14a
출처 데이터셋
uspto-grants-2009_05
특허 번호
US07538123B2

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