Methylglyoxal → 2-Methyl-6-fluoroquinoxaline

HRID 1189192ノート

反応式

HRID 1189192 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-1688e76b73fe45bfa8c06307a6cc6c20
出典データセット
uspto-grants-2014_03
特許番号
US08674106B2

反応ノート

読み込み中…