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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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HCID 178524696, 화합물 → HCID 66629888, 화합물

HRID 1825768
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HRID 1825768 반응식
[OH:1][C:2]1[C:11]2[C:6](=[CH:7][C:8]3[O:14][CH2:13][O:12][C:9]=3[CH:10]=2)[N:5]=[CH:4][C:3]=1C(O)=O>C1(OC2C=CC=CC=2)C=CC=CC=1>[CH2:13]1[O:14][C:8]2[CH:7]=[C:6]3[C:11]([C:2](=[O:1])[CH2:3][CH:4]=[N:5]3)=[CH:10][C:9]=2[O:12]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 1

HCID 178524696HCID 178524696, 화합물

생성물 1

HCID 66629888HCID 66629888, 화합물

시약·촉매·용매 1

HCID 7583Diphenyl Ether용매

실험 절차

A suspension of 4-hydroxy-6,7-methylenedioxy-3-quinolinecarboxylic acid (30 g, 0.129 mol) in diphenyl ether (320 mL) was heated to reflux with vigorous stirring. The reaction was carefully monitored until it became clear, about 1.5 h, and then immediately removed from heat. By this time all of the starting material had dissolved but a black tarry residue remained. The solution was decanted and cooled, allowing the product to precipitate. This material was filtered and washed with ethyl ether to remove all traces of phenyl ether. A second crop was obtained by vigorously washing the tarry residue with ethanol (16×250 mL), filtering and evaporating the ethanol, and rinsing the material with ethyl ether. The total yield was 14.9 g as a pale yellow solid, in 61%; mp 285-289° C. (lit.221 mp 276° C.); 1H NMR (DMSO-d6) δ 5.95 (d, 1H, J=7.3), 6.13 (s, 2H), 6.97 (s, 1H), 7.38 (s, 1H), 7.77 (d, 1H, J=7.3); 13C NMR (DMSO-d6) δ 97.5, 102.1, 102.6, 108.7, 119.4, 122.0, 130.8, 138.7, 145.8, 151.7.

후처리

  1. temperaturewas heated
  2. temperatureto reflux with vigorous stirring
  3. customimmediately removed
  4. temperaturefrom heat
  5. dissolutionBy this time all of the starting material had dissolved
  6. customThe solution was decanted
  7. temperaturecooled
  8. customto precipitate
  9. filtrationThis material was filtered
  10. washwashed with ethyl ether
  11. customto remove all traces of phenyl ether
  12. customA second crop was obtained
  13. washby vigorously washing the tarry residue with ethanol (16×250 mL)
  14. filtrationfiltering
  15. customevaporating the ethanol
  16. washrinsing the material with ethyl ether

출처 및 근거

ORD 기록
ord-6621ebed6f3e433780ec7d030c744a18
출처 데이터셋
uspto-grants-2006_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07049315B2

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