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Tetrahydrofuran → 6,7-Dichloro-2,3-dimethoxy-5-methylquinoxaline

HRID 1957120
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반응식

HRID 1957120 반응식
[CH3:1][O-:2].[Na+].[CH3:4][C:5]1[C:14]([Cl:15])=[C:13]([Cl:16])[CH:12]=[C:11]2[C:6]=1[N:7]=[C:8](Cl)[C:9](Cl)=[N:10]2.[O:19]1[CH2:23]CCC1>C(OCC)(=O)C>[Cl:15][C:14]1[C:5]([CH3:4])=[C:6]2[C:11](=[CH:12][C:13]=1[Cl:16])[N:10]=[C:9]([O:2][CH3:1])[C:8]([O:19][CH3:23])=[N:7]2
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참가 물질

5

반응물 3

HCID 8028TetrahydrofuranHCID 106781235-Methyl-2,3,6,7-tetrachloroquinoxalineHCID 10942334Sodium Methoxide

생성물 1

HCID 108021936,7-Dichloro-2,3-dimethoxy-5-methylquinoxaline수율 100%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

A solution of sodium methoxide (38 mL , 25% solution in methanol, 175 mmol) was added over 10 minutes to a solution of 5-methyl-2,3,6,7-tetrachloroquinoxaline (21 g, 74 mmol) in dry tetrahydrofuran (200 mL) at 20° C. There was a mildly exothermic reaction followed by formation of a precipitate. After 1 hour the mixture was diluted with ethyl acetate (3 L), washed with water (1 L), dried (MgSO4) and concentrated under reduced pressure to give 6,7dichloro-2,3-dimethoxy-5-methylquinoxaline (20.3 g, 100%).

후처리

  1. customa mildly exothermic reaction
  2. washwashed with water (1 L)
  3. dry with materialdried (MgSO4)
  4. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-b6140550907a4238ad288eedf7220992
출처 데이터셋
uspto-grants-1998_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05783572

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