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Potassium Carbonate → HCID 21270184、化合物

HRID 1194473
ノート
印刷プレビュー

反応式

HRID 1194473 の反応式
[OH:1][C:2]1[CH:19]=[CH:18][C:5]2[C:6](=[O:17])[C:7]([C:10]3[CH:15]=[CH:14][C:13]([CH3:16])=[CH:12][CH:11]=3)=[CH:8][O:9][C:4]=2[C:3]=1O.[C:21](=[O:24])([O-])[O-].[K+].[K+].S([O-])(O[CH3:31])(=O)=O>CC(C)=O>[CH3:31][O:1][C:2]1[CH:19]=[CH:18][C:5]2[C:6](=[O:17])[C:7]([C:10]3[CH:15]=[CH:14][C:13]([CH3:16])=[CH:12][CH:11]=3)=[CH:8][O:9][C:4]=2[C:3]=1[O:24][CH3:21]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 4694097Methyl sulfate(1-)HCID 5481241HCID 5481241、化合物

生成物 1

HCID 21270184HCID 21270184、化合物

試薬・触媒・溶媒 1

HCID 180Acetone溶媒2 回

実験手順

7,8-Dihydroxy-3-(4-methylphenyl)-4H-1-benzopyran-4-one (2.7 g), described in example 9, is dissolved in dry acetone (50 ml). Pyrolyzed potassium carbonate (4.14 g) is added and the mixture is heated to reflux. A solution of methyl sulphate (3.78 g) in acetone (10 ml) is then added dropwise and heating is maintained for three more hours. After cooling, the solid is filtered and the solution is evaporated to dryness under vacuum. Water is added to the residue which is filtered, washed with an aqueous sodium hydroxide solution (1N) then with water and dried. After crystallization in methanol, 7,8-dimethoxy-3-(4-methylphenyl)-4H-1-benzopyran-4-one is obtained, m.p. 135°.

後処理

  1. temperaturethe mixture is heated to reflux
  2. temperatureheating
  3. temperatureis maintained for three more hours
  4. temperatureAfter cooling
  5. filtrationthe solid is filtered
  6. customthe solution is evaporated to dryness under vacuum
  7. additionWater is added to the residue which
  8. filtrationis filtered
  9. washwashed with an aqueous sodium hydroxide solution (1N)
  10. dry with materialwith water and dried
  11. customAfter crystallization in methanol

出典と根拠

ORDレコード
ord-2b5b1880c66d49e893a283b139f4345a
出典データセット
uspto-grants-1989_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04814346

反応ノート

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