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Hydrochloric Acid → HCID 13288097、化合物

HRID 1981919
ノート
印刷プレビュー

反応式

HRID 1981919 の反応式
[CH2:1]([O:3][C:4]1[CH:24]=[CH:23][CH:22]=[CH:21][C:5]=1[C:6]1[O:7][C:8]2[C:13]([C:14](=[O:17])[C:15]=1[CH3:16])=[CH:12][CH:11]=[CH:10][C:9]=2[C:18]([OH:20])=[O:19])[CH3:2].C(=O)([O-])[O-].[K+].[K+].[CH2:31](Br)[CH2:32][OH:33].Cl>CN(C)C=O>[CH2:1]([O:3][C:4]1[CH:24]=[CH:23][CH:22]=[CH:21][C:5]=1[C:6]1[O:7][C:8]2[C:13]([C:14](=[O:17])[C:15]=1[CH3:16])=[CH:12][CH:11]=[CH:10][C:9]=2[C:18]([O:20][CH2:31][CH2:32][OH:33])=[O:19])[CH3:2]
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 313Hydrochloric AcidHCID 108982-BromoethanolHCID 11430Potassium CarbonateHCID 132881092-(2-Ethoxyphenyl)-3-methyl-4-oxo-4H-1-benzopyran-8-carboxylic acid

生成物 1

HCID 13288097HCID 13288097、化合物収率 70.4%

試薬・触媒・溶媒 1

HCID 6228
Dimethylformamide
溶媒

実験手順

One gram of 2'-ethoxy-3-methylflavone-8-carboxylic acid prepared by the same way as Example 1 is dissolved in 30 ml of dimethyl formamide, 0.5 gram of anhydrous potassium carbonate is added thereto, 2 grams of ethylene bromohydrin is dropped thereinto with stirring, and the mixture is stirred at 50° C. for four hours. Then it is poured into ice water, the mixture is neutralized with 10% hydrochloric acid, extracted with ethyl acetate, the extract is washed with water, dried with anhydrous magnesium sulfate, the solvent is evaporated therefrom, and the residue is recrystallized from a mixture of benzene and n-hexane to give 0.8 gram of beta-hydroxyethyl 2'-ethoxy-3-methylflavone-8-carboxylate, colorless needles, melting point 143° to 144.5° C.

後処理

  1. stirringthe mixture is stirred at 50° C. for four hours
  2. extractionextracted with ethyl acetate
  3. washthe extract is washed with water
  4. dry with materialdried with anhydrous magnesium sulfate
  5. customthe solvent is evaporated
  6. customthe residue is recrystallized from a mixture of benzene and n-hexane

出典と根拠

ORDレコード
ord-ffe9e69e1d504aa9a4cb4ccd8a8cacec
出典データセット
uspto-grants-1986_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04594345

反応ノート

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