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Potassium Hydroxide → HCID 178524696、化合物

HRID 505878
ノート
印刷プレビュー

反応式

HRID 505878 の反応式
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]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

HCID 178524696HCID 178524696、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-7f3e4c815930414bb06361a1ce835eac
出典データセット
uspto-grants-2010_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07781587B2

反応ノート

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