Pyridinium chloride → 3-(2,4-Dihydroxyphenyl)-7-hydroxy-4-methyl-chromen-2-one

HRID 2055031

反応式

HRID 2055031 の反応式
C[O:2][C:3]1[CH:8]=[C:7]([O:9]C)[CH:6]=[CH:5][C:4]=1[CH:11]1[C:20]([CH3:21])=[C:19]2[C:14](=[CH:15][C:16](OC(=O)C)([OH:22])[CH:17]=[CH:18]2)[O:13][C:12]1=[O:27].Cl.N1C=CC=CC=1>>[OH:2][C:3]1[CH:8]=[C:7]([OH:9])[CH:6]=[CH:5][C:4]=1[C:11]1[C:12](=[O:27])[O:13][C:14]2[C:19]([C:20]=1[CH3:21])=[CH:18][CH:17]=[C:16]([OH:22])[CH:15]=2

参加物

3

反応物 2

HCID 10176127Pyridinium chlorideHCID 69317693Acetic acid 3-(2,4-dimethoxyphenyl)-7-hydroxy4-methyl-2-oxo-2H-chromen-7-yl ester

生成物 1

HCID 111968603-(2,4-Dihydroxyphenyl)-7-hydroxy-4-methyl-chromen-2-one

反応条件

温度
210 °C

実験手順

A mixture of acetic acid 3-(2,4-dimethoxyphenyl)-7-hydroxy-4-methyl-2-oxo-2H-chromen-7-yl ester, prepared as in Example 1 (0.177 g, 0.5 mmol, 1 eq) and dry pyridine hydrochloride (0.9 g, 8.8 mmol, 16 eq) was stirred and heated in an oil bath to a melt, at 210° C. under a closed nitrogen atmosphere in a loosely stoppered round bottom flask for 1 hour. After cooling to room temperature the reaction mixture was triturated with water and the aqueous solution was extracted several times with ethyl acetate until the latter was colorless. Combined organic extracts were washed with brine, dried (anhydrous sodium sulphate), filtered and evaporated to yield the title compound as a pinkish crystalline solid.

後処理

  1. temperatureAfter cooling to room temperature the reaction mixture
  2. customwas triturated with water
  3. extractionthe aqueous solution was extracted several times with ethyl acetate until the latter
  4. washCombined organic extracts were washed with brine
  5. dry with materialdried (anhydrous sodium sulphate)
  6. filtrationfiltered
  7. customevaporated

出典と根拠

ORDレコード
ord-2403278804b54816b7ec9dc1a20c1c45
出典データセット
uspto-grants-2008_02
特許番号
US07329654B2

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