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Water → HCID 86725012、化合物

HRID 1847088
ノート
印刷プレビュー

反応式

HRID 1847088 の反応式
[H-].[Li+].[F:3][C:4]1[CH:13]=[C:12]2[C:7]([N:8]=[CH:9][C:10](=[O:14])[NH:11]2)=[CH:6][CH:5]=1.Br[CH2:16][CH2:17][CH:18]1[O:22][CH2:21][CH2:20][O:19]1.O>CN(C)C=O>[O:19]1[CH2:20][CH2:21][O:22][CH:18]1[CH2:17][CH2:16][N:11]1[C:12]2[C:7](=[CH:6][CH:5]=[C:4]([F:3])[CH:13]=2)[N:8]=[CH:9][C:10]1=[O:14]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 62714Lithium hydrideHCID 877762-(2-Bromoethyl)-1,3-dioxolaneHCID 217275347-fluoroquinoxalin-2(1H)-one

生成物 1

HCID 86725012HCID 86725012、化合物収率 29.1%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

Lithium hydride (88 mg, 011 mmol) was added to a solution of 7-fluoroquinoxalin-2(1H)one (1.3 g, 7.8 mmol) in N,N-dimethylformamide (40 ml) under cooling on ice and the mixture was stirred at room temperature for 30 minutes. The mixture was cooled on ice and 2-(2-bromoethyl)-1,3-dioxolane (1.33 ml, 11 mmol) was added thereto. The obtained mixture was stirred at room temperature for 24 hours, water was then gradually added thereto and the mixture was extracted with ethyl acetate. The organic layer was dried over anhydrous sodium sulfate and concentrated under reduced pressure. The obtained crude product was purified by silica gel column chromatography (dichloromethane/methanol) to yield 0.6 g (29%) of the title compound.

後処理

  1. temperatureunder cooling on ice
  2. additionwas added
  3. stirringThe obtained mixture was stirred at room temperature for 24 hours
  4. extractionthe mixture was extracted with ethyl acetate
  5. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  6. concentrationconcentrated under reduced pressure
  7. customThe obtained crude product
  8. customwas purified by silica gel column chromatography (dichloromethane/methanol)

出典と根拠

ORDレコード
ord-4377bf453226494d9f1e44aa5a04d88a
出典データセット
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08952010B2

反応ノート

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