Hydrochloric Acid → 5-Methoxy-2-(3-methylbut-2-enyloxy)benzaldehyde

HRID 30093

反応式

HRID 30093 の反応式
[OH:1][C:2]1[CH:9]=[CH:8][C:7]([O:10][CH3:11])=[CH:6][C:3]=1[CH:4]=[O:5].C(=O)([O-])[O-].[K+].[K+].Br[CH2:19][CH:20]=[C:21]([CH3:23])[CH3:22].Cl>CN(C)C=O.C(OCC)(=O)C>[CH3:11][O:10][C:7]1[CH:8]=[CH:9][C:2]([O:1][CH2:19][CH:20]=[C:21]([CH3:23])[CH3:22])=[C:3]([CH:6]=1)[CH:4]=[O:5]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 700922-Butene, 1-bromo-3-methyl-HCID 956952-Hydroxy-5-methoxybenzaldehyde

生成物 1

HCID 105849975-Methoxy-2-(3-methylbut-2-enyloxy)benzaldehyde

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of 2-hydroxy-5-methoxybenzaldehyde (7.6 g, 50 mmol) in dry N,N-dimethylformamide (100 mL) was added potassium carbonate (10.4 g), followed by 1-bromo-3-methylbut-2-ene (10.0 g, 67 mmol). The mixture was stirred at room temperature for 48 hours and ethyl acetate added. Sufficient 1M hydrochloric acid was cautiously added to neutralize the base, and the organic layer was washed with water three times, followed by brine, and dried over magnesium sulfate. The mixture was filtered, and solvent removed from the filtrate under reduced pressure, to provide 5-methoxy-2-(3 -methylbut-2-enyloxy)benzaldehyde.

後処理

  1. washthe organic layer was washed with water three times
  2. dry with materialdried over magnesium sulfate
  3. filtrationThe mixture was filtered
  4. customsolvent removed from the filtrate under reduced pressure

出典と根拠

ORDレコード
ord-06f988e364c540fbacba7f1878f5c21d
出典データセット
uspto-grants-2008_09
特許番号
US07423045B2

関連ノート

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