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Quinoline → HCID 178516363、化合物

HRID 1579915
ノート
印刷プレビュー

反応式

HRID 1579915 の反応式
[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.N1C2C(=CC=CC=2)C=CC=1>CCOCC>[CH2:13]1[O:14][C:8]2[CH:7]=[C:6]3[C:11]([C:2]([OH:1])=[CH:3][CH:4]=[N:5]3)=[CH:10][C:9]=2[O:12]1
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 7047QuinolineHCID 178524696HCID 178524696、化合物

生成物 1

HCID 178516363HCID 178516363、化合物

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

A suspension of 50 g. of 4-hydroxy-6,7-methylenedioxyquinoline-3-carboxylic acid in 500 ml. of freshly distilled quinoline was heated at 200° until the evolution of gas ceased. The reaction mixture was cooled to room temperature, diluted with an equal amount of ether and kept cool overnight. The precipitated brown solid (51.4 g., m.p. 254°-267°) was collected by filtration and dissolved in refluxing ethanol. The insoluble material was removed and the ethanol solution was reduced to one-third of its volume. The solution was diluted with an equal amount of ether. On cooling, 31.1 g. of 6,7-methylenedioxy-4-quinolinol separated, m.p. 280°-282°. Recrystallization (2x) from hot water yielded analytically pure 6,7-methylenedioxy-4-quinolinol as a pale yellow solid, m.p. 288°-289°.

後処理

  1. additionA suspension of 50 g
  2. temperaturekept cool overnight
  3. filtrationThe precipitated brown solid (51.4 g., m.p. 254°-267°) was collected by filtration
  4. dissolutiondissolved
  5. temperaturein refluxing ethanol
  6. customThe insoluble material was removed
  7. additionThe solution was diluted with an equal amount of ether
  8. temperatureOn cooling
  9. customof 6,7-methylenedioxy-4-quinolinol separated
  10. customRecrystallization (2x) from hot water

出典と根拠

ORDレコード
ord-ecdb335288d447f5aeca6ccf15fd77d6
出典データセット
uspto-grants-1976_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03931193

反応ノート

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