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Methyl iodide → HCID 58909275、化合物

HRID 1985090
ノート
印刷プレビュー

反応式

HRID 1985090 の反応式
[CH2:1]([C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[NH:9][CH2:8][CH2:7][C:6]2=[O:13])[CH3:2].[CH2:14](N(CC)CC)C.IC>C1COCC1>[CH2:1]([C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[N:9]([CH3:14])[CH2:8][CH2:7][C:6]2=[O:13])[CH3:2]
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 6328Methyl iodideHCID 8471TriethylamineHCID 223244436-Ethyl-2,3-dihydroquinolin-4(1H)-one

生成物 1

HCID 58909275HCID 58909275、化合物収率 30%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
70 °C

実験手順

To a solution of 6-ethyl-2,3-dihydroquinolin-4(1H)-one (1.00 g) in THF (25 mL) was added triethylamine (0.64 g) followed by iodomethane (0.89 g). The mixture was refluxed at 70° C. overnight. The solvent was stripped under reduced pressure, and the residue was partitioned between aqueous sodium bicarbonate and dichloromethane. The organics were extracted three times, washed with brine, dried with sodium sulfate, filtered, and concentrated. Chromatography was used to purify the title compound using a 40% ethyl acetate in heptane solvent solution. 0.32 g of the title product were recovered. (30% yield). MS (ESI+) for C12H15NO m/z 190.10 (M+H)+.

後処理

  1. customthe residue was partitioned between aqueous sodium bicarbonate and dichloromethane
  2. extractionThe organics were extracted three times
  3. washwashed with brine
  4. dry with materialdried with sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customto purify the title compound
  8. custom0.32 g of the title product were recovered

出典と根拠

ORDレコード
ord-200443c249654297ad96600b7ffa3488
出典データセット
uspto-grants-2009_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07544717B2

反応ノート

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