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Potassium Carbonate → HCID 14329994, 화합물

HRID 2231465
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HRID 2231465 반응식
[Cl:1][C:2]1[C:3]([OH:15])=[C:4]([CH2:12][CH2:13][CH3:14])[C:5]([OH:11])=[C:6]([C:8](=[O:10])[CH3:9])[CH:7]=1.[CH3:16][O:17][C:18](=[O:38])[CH2:19][O:20][C:21]1[CH:26]=[CH:25][C:24]([C:27](=[O:29])[CH3:28])=[C:23]([O:30][CH2:31][CH2:32][CH2:33]Br)[C:22]=1[CH2:35][CH2:36][CH3:37].C(=O)([O-])[O-].[K+].[K+]>CC(C)=O>[CH3:16][O:17][C:18](=[O:38])[CH2:19][O:20][C:21]1[CH:26]=[CH:25][C:24]([C:27](=[O:29])[CH3:28])=[C:23]([O:30][CH2:31][CH2:32][CH2:33][O:15][C:3]2[C:2]([Cl:1])=[CH:7][C:6]([C:8](=[O:10])[CH3:9])=[C:5]([OH:11])[C:4]=2[CH2:12][CH2:13][CH3:14])[C:22]=1[CH2:35][CH2:36][CH3:37]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11430Potassium Carbonate2회HCID 133891721-(5-Chloro-2,4-dihydroxy-3-propylphenyl)ethanoneHCID 53783998HCID 53783998, 화합물

생성물 1

HCID 14329994HCID 14329994, 화합물수율 58%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

A mixture of 2 g (0.0088 mol) of 1-(5-chloro-2,4-dihydroxy-3-propylphenyl)ethanone, 3.39 g (0.0088 mol) of [4-acetyl-3-(3-bromopropoxy)-2-propylphenoxy]acetic acid methyl ester and 1.8 g (0.013 mol) of anhydrous potassium carbonate in 150 ml of anhydrous acetone was stirred at reflux for 20 hours. An additional 1.0 g of potassium carbonate was added and reflux was continued for a total of 35 hours. The hot reaction mixture was filtered and filtrate was concentrated in vacuo to an oil which was dissolved in ethyl acetate and washed with 1N sodium hydroxide and sodium chloride solution. The crude oil obtained on concentration of the ethyl acetate solution was purified by HPLC, eluting with 30% ethyl acetate in hexane to yield 2.7 g (58% yield) of [4-acetyl-3-[3-(4-acetyl-6-chloro-3-hydroxy-2-propylphenoxy)propoxy]-2-propylphenoxy]acetic acid methyl ester as a pale yellow oil.

후처리

  1. temperatureat reflux for 20 hours
  2. temperaturereflux
  3. customwas continued for a total of 35 hours
  4. filtrationThe hot reaction mixture was filtered
  5. concentrationfiltrate was concentrated in vacuo to an oil which
  6. dissolutionwas dissolved in ethyl acetate
  7. washwashed with 1N sodium hydroxide and sodium chloride solution
  8. customThe crude oil obtained on concentration of the ethyl acetate solution
  9. customwas purified by HPLC
  10. washeluting with 30% ethyl acetate in hexane

출처 및 근거

ORD 기록
ord-10924feeb46a42c9b46351bc97d94ba4
출처 데이터셋
uspto-grants-1988_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04782176

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