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Water → 2-[6-Methoxy-4-(2-methyl-quinolin-3-yloxy)-quinolin-7-yloxy]-propane-1,3-diol

HRID 228974
ノート
印刷プレビュー

反応式

HRID 228974 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:12]=1[O:13][CH:14]([C:20](OCC)=[O:21])[C:15](OCC)=[O:16])[N:9]=[CH:8][CH:7]=[C:6]2[O:25][C:26]1[C:27]([CH3:36])=[N:28][C:29]2[C:34]([CH:35]=1)=[CH:33][CH:32]=[CH:31][CH:30]=2.[H-].[Al+3].[Li+].[H-].[H-].[H-].O>O1CCCC1>[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:12]=1[O:13][CH:14]([CH2:20][OH:21])[CH2:15][OH:16])[N:9]=[CH:8][CH:7]=[C:6]2[O:25][C:26]1[C:27]([CH3:36])=[N:28][C:29]2[C:34]([CH:35]=1)=[CH:33][CH:32]=[CH:31][CH:30]=2
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 962WaterHCID 21226445Aluminium lithium hydrideHCID 57756541Diethyl 2-[6-methoxy-4-(2-methyl-quinolin-3-yloxy)-quinolin-7-yloxy]-malonate2 回

生成物 1

HCID 577564172-[6-Methoxy-4-(2-methyl-quinolin-3-yloxy)-quinolin-7-yloxy]-propane-1,3-diol収率 22%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
0 °C

実験手順

Diethyl 2-[6-methoxy-4-(2-methyl-quinolin-3-yloxy)-quinolin-7-yloxy]-malonate (compound 373) (50 mg) was dissolved in tetrahydrofuran (1 ml) to prepare a solution. Lithium aluminum hydride (10 mg) was added to the solution at 0° C., and the mixture was stirred at 0° C. for 3 hr and then at room temperature for 2 hr. Water was added to the reaction solution to stop the reaction. The mixture was filtered through Celite, water was then added to the filtrate, and the mixture was extracted with chloroform. The chloroform layer was washed with water and was then dried over anhydrous sodium sulfate. The solvent was removed by distillation under the reduced pressure, and the residue was purified by thin layer chromatography using chloroform-methanol to give the title compound (9.1 mg, yield 22%).

後処理

  1. customto prepare a solution
  2. waitat room temperature for 2 hr
  3. customthe reaction
  4. filtrationThe mixture was filtered through Celite, water
  5. additionwas then added to the filtrate
  6. extractionthe mixture was extracted with chloroform
  7. washThe chloroform layer was washed with water
  8. dry with materialwas then dried over anhydrous sodium sulfate
  9. customThe solvent was removed by distillation under the reduced pressure
  10. customthe residue was purified by thin layer chromatography

出典と根拠

ORDレコード
ord-69c76b390f694a5a9942e93b6260f91c
出典データセット
uspto-grants-2009_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07560558B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート