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

HRID 1981242
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HRID 1981242 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 7918Acetic AnhydrideHCID 8857Ethyl Acetate2회HCID 13377328HCID 13377328, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-675d917e39ce42ae8b450e3dd944ac33
출처 데이터셋
uspto-grants-1985_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04513145

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