Dimethylformamide → HCID 89586186、化合物

HRID 1747775ノート

反応式

HRID 1747775 の反応式
[C:1]([C:4]1[O:5][C:6]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)=[CH:7][C:8](=[O:11])[C:9]=1[OH:10])(=[O:3])[CH3:2].[C:18](=O)([O-])[O-].[K+].[K+].IC.CN(C=O)C>O>[C:1]([C:4]1[O:5][C:6]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)=[CH:7][C:8](=[O:11])[C:9]=1[O:10][CH3:18])(=[O:3])[CH3:2]

参加物

6

反応物 4

HCID 6228DimethylformamideHCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 132009232-Acetyl-3-hydroxy-6-phenyl-4H-pyran-4-one

生成物 1

HCID 89586186HCID 89586186、化合物収率 42.4%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of 2-acetyl-3-hydroxy-6-phenyl-4H-pyran-4-one (200 mg), potassium carbonate (150 mg), iodomethane (0.0600 mL) and DMF (5.0 mL) was stirred at room temperature overnight. The reaction mixture was diluted with water and the mixture was extracted with ethyl acetate. The extract was dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/hexane) to give the title compound (90.0 mg).

後処理

  1. extractionthe mixture was extracted with ethyl acetate
  2. dry with materialThe extract was dried over anhydrous sodium sulfate
  3. concentrationconcentrated under reduced pressure
  4. customThe residue was purified by silica gel column chromatography (ethyl acetate/hexane)

出典と根拠

ORDレコード
ord-d92a07a2721e42a08216311e32d3366b
出典データセット
uspto-grants-2015_10
特許番号
US09150588B2

反応ノート

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