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Potassium Hydroxide → HCID 178524696, 화합물

HRID 1825767
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HRID 1825767 반응식
C([O:3][C:4]([C:6]1[CH:7]=[N:8][C:9]2[C:14]([C:15]=1[OH:16])=[CH:13][C:12]1[O:17][CH2:18][O:19][C:11]=1[CH:10]=2)=[O:5])C.[OH-].[K+]>C(O)C>[OH:16][C:15]1[C:14]2[C:9](=[CH:10][C:11]3[O:19][CH2:18][O:17][C:12]=3[CH:13]=2)[N:8]=[CH:7][C:6]=1[C:4]([OH:5])=[O:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 14797Potassium HydroxideHCID 84257Ethyl 8-hydroxy-(1,3)dioxolo(4,5-g)quinoline-7-carboxylate

생성물 1

HCID 178524696HCID 178524696, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

4-Hydroxy-6,7-methylenedioxy-3-quinolinecarboxylic acid ethyl ester (45.0 g, 0.172 mol) was added to a solution of KOH (16.8 g, 0.258 mol) in ethanol (500 mL) and the mixture was heated to reflux with stirring for 20 hours. The reaction flask was then cooled and ethanol was evaporated under reduced pressure. Then 800 mL of water were added with stirring to fully dissolve the potassium salt, and the solution was filtered to remove any impurities. Concentrated HCl was added to bring the mixture to pH 1, and the free acid was filtered off and dried under vacuum, to give 33.9 g as a beige solid, in 84%; mp >300° C. (lit.221 mp >290° C.); 1H NMR (DMSO-d6) δ 6.27 (s, 2H), 7.30 (s, 1H), 7.55 (s, 1H), 8.72 (s, 1H); 13C NMR (DMSO-d6) δ 98.5, 101.8, 103.8, 107.9, 120.8, 137.9, 143.5, 148.1, 153.7, 167.4, 177.4.

후처리

  1. temperaturethe mixture was heated
  2. temperatureto reflux
  3. temperatureThe reaction flask was then cooled
  4. customethanol was evaporated under reduced pressure
  5. additionThen 800 mL of water were added
  6. stirringwith stirring
  7. dissolutionto fully dissolve the potassium salt
  8. filtrationthe solution was filtered
  9. customto remove any impurities
  10. additionConcentrated HCl was added
  11. filtrationthe free acid was filtered off
  12. customdried under vacuum
  13. customto give 33.9 g as a beige solid

출처 및 근거

ORD 기록
ord-be9b1251602c4bfaaf9a658f1d61bd53
출처 데이터셋
uspto-grants-2006_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07049315B2

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