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Dimethylformamide → 6,7-Bis(acetyloxy)-2-methyl-4-oxo-4H-1-benzopyran-3-carboxylic acid

HRID 1981242
ノート
印刷プレビュー

反応式

HRID 1981242 の反応式
[OH:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][C:11]=1[OH:12])[O:8][C:7]([CH3:13])=[C:6]([C:14]([OH:16])=[O:15])[C:5]2=[O:17].CN(C)C=O.[C:23](OC(=O)C)(=[O:25])[CH3:24].[C:30](OCC)(=[O:32])[CH3:31]>N1C=CC=CC=1>[C:23]([O:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][C:11]=1[O:12][C:30](=[O:32])[CH3:31])[O:8][C:7]([CH3:13])=[C:6]([C:14]([OH:16])=[O:15])[C:5]2=[O:17])(=[O:25])[CH3:24]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 6228DimethylformamideHCID 7918Acetic AnhydrideHCID 8857Ethyl Acetate2 回HCID 13377328HCID 13377328、化合物

生成物 1

HCID 134585256,7-Bis(acetyloxy)-2-methyl-4-oxo-4H-1-benzopyran-3-carboxylic acid

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

A mixture of 6,7-dihydroxy-2-methylchromone-3-carboxylic acid (2.24 g), dimethylformamide (30 ml), ethyl acetate (10 ml), pyridine (2.3 ml) and acetic anhydride (2.3 ml) was stirred at room temperature for 3 hours. Ethyl acetate (100 ml) was added to the reaction mixture, and the organic layer was washed successively with 6N-HCl and water, and thereafter dried over anhydrous magnesium sulfate. The solvent was evaporated and ethyl ether was added to the residue. The resulting solid was collected by filtration. It was washed with a 1:1 mixed solvent of ethyl acetate and ethyl ether and then dried, to obtain the desired product (1.93 g).

後処理

  1. washthe organic layer was washed successively with 6N-HCl and water
  2. dry with materialdried over anhydrous magnesium sulfate
  3. customThe solvent was evaporated
  4. additionethyl ether was added to the residue
  5. filtrationThe resulting solid was collected by filtration
  6. washIt was washed with a 1:1 mixed solvent of ethyl acetate and ethyl ether
  7. customdried

出典と根拠

ORDレコード
ord-675d917e39ce42ae8b450e3dd944ac33
出典データセット
uspto-grants-1985_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04513145

反応ノート

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