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Hydrochloric Acid → HCID 13288097, 화합물

HRID 1981919
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HRID 1981919 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 108982-BromoethanolHCID 11430Potassium CarbonateHCID 132881092-(2-Ethoxyphenyl)-3-methyl-4-oxo-4H-1-benzopyran-8-carboxylic acid

생성물 1

HCID 13288097HCID 13288097, 화합물수율 70.4%

시약·촉매·용매 1

HCID 6228
Dimethylformamide
용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-ffe9e69e1d504aa9a4cb4ccd8a8cacec
출처 데이터셋
uspto-grants-1986_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04594345

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