Water → 2-Allyloxy-4-methoxynitrobenzene

HRID 494919

反応式

HRID 494919 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]([N+:10]([O-:12])=[O:11])=[C:7]([OH:9])[CH:8]=1.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:9][C:7]1[CH:8]=[C:3]([O:2][CH3:1])[CH:4]=[CH:5][C:6]=1[N+:10]([O-:12])=[O:11])[CH:20]=[CH2:19]

参加物

7

反応物 4

HCID 962WaterHCID 7841Allyl bromideHCID 11430Potassium CarbonateHCID 2196355-Methoxy-2-nitrophenol

生成物 1

HCID 103307082-Allyloxy-4-methoxynitrobenzene

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

1.88 g of 5-methoxy-2-nitrophenol was dissolved in 20 ml of N,N-dimethylformamide. Thereafter, 1.53 g of potassium carbonate and 1.03 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 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 2.09 g of the subject compound.

後処理

  1. customso as to separate an organic layer
  2. washThe obtained organic layer was washed with water
  3. dry with materiala saturated sodium chloride 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)

出典と根拠

ORDレコード
ord-b7264fe89c7f4f57b1191361e76af406
出典データセット
uspto-grants-2009_05
特許番号
US07538123B2

関連ノート

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