Methylglyoxal → 2-Methyl-6-fluoroquinoxaline

HRID 1189192노트

반응식

HRID 1189192 반응식
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

참가 물질

4

반응물 2

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

생성물 1

HCID 133808502-Methyl-6-fluoroquinoxaline수율 80%

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-1688e76b73fe45bfa8c06307a6cc6c20
출처 데이터셋
uspto-grants-2014_03
특허 번호
US08674106B2

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