Methylglyoxal → 2-Methyl-6-fluoroquinoxaline

HRID 422385ノート

反応式

HRID 422385 の反応式
O=[C:2]([CH3:5])[CH:3]=O.[F:6][C:7]1[CH:8]=[C:9]([NH2:14])[C:10]([NH2:13])=[CH:11][CH:12]=1>O>[F:6][C:7]1[CH:8]=[C:9]2[C:10](=[CH:11][CH:12]=1)[N:13]=[C:2]([CH3:5])[CH:3]=[N:14]2

参加物

4

反応物 2

HCID 880MethylglyoxalHCID 1645844-Fluorobenzene-1,2-diamine

生成物 1

HCID 133808502-Methyl-6-fluoroquinoxaline収率 80%

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

A solution of 2-oxo-propionaldehyde (0.19 mL, 1.20 mmol) and 4-fluoro-benzene-1,2-diamine (150 mg, 1.19 mmol) in water (1.3 mL) was placed in a microwave tube and heated for 1 min at 150 W. Then the reaction mixture was diluted with water and extracted twice with AcOEt. The organic phase was washed with water, brine, dried over MgSO4, filtered and evaporated. The crude residue was purified by flash chromatography (cyclohexane/AcOEt 4:1) to yield 154 mg (0.95 mmol; 80%) of 6-fluoro-2-methyl-quinoxaline.

後処理

  1. temperatureheated for 1 min at 150 W
  2. extractionextracted twice with AcOEt
  3. washThe organic phase was washed with water, brine
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. customevaporated
  7. customThe crude residue was purified by flash chromatography (cyclohexane/AcOEt 4:1)

出典と根拠

ORDレコード
ord-62208cdc0e014334bcc4ee0a817468e1
出典データセット
uspto-grants-2012_01
特許番号
US08101637B2

反応ノート

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