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Dichloromethane → 2-(3-Chloro-2,5,6-trifluoropyridin-4-yl)-1H-isoindole-1,3(2H)-dione

HRID 1274721
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HRID 1274721 반응식
ClCCl.[Cl:4][C:5]1[C:6]([F:14])=[N:7][C:8]([F:13])=[C:9]([F:12])[C:10]=1F.[C:15]1(=[O:25])[NH:19][C:18](=[O:20])[C:17]2=[CH:21][CH:22]=[CH:23][CH:24]=[C:16]12.[K]>C(Cl)(Cl)Cl>[Cl:4][C:5]1[C:6]([F:14])=[N:7][C:8]([F:13])=[C:9]([F:12])[C:10]=1[N:19]1[C:18](=[O:20])[C:17]2=[CH:21][CH:22]=[CH:23][CH:24]=[C:16]2[C:15]1=[O:25]
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참가 물질

5

반응물 3

HCID 6344DichloromethaneHCID 1371833-Chloro-2,4,5,6-tetrafluoropyridineHCID 24194345Phthalimide potassium salt

생성물 1

HCID 221212012-(3-Chloro-2,5,6-trifluoropyridin-4-yl)-1H-isoindole-1,3(2H)-dione수율 102.6%

시약·촉매·용매 1

HCID 6212Chloroform용매

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온도
40 °C

실험 절차

To a mixed solution of 40 ml dichloromethane and 20 ml N,N-methylformamide were added 18.5 g of 3-chloro-2,4,5,6-tetrafluoropyridine and 20.5 g potassium phthalimide, and the mixture was stirred at 40° C. for one day. After adding 40 ml of chloroform, the mixture was washed twice with 500 ml of distilled water and once with 500 ml of 0.5% aqueous solution of sodium hydroxide. The organic layer was dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The precipitate was dispersed in diisopropylether, and collected by filtration to obtain 32.0 g of the title compound as a colorless powder.

후처리

  1. washthe mixture was washed twice with 500 ml of distilled water and once with 500 ml of 0.5% aqueous solution of sodium hydroxide
  2. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  3. concentrationconcentrated under reduced pressure
  4. additionThe precipitate was dispersed in diisopropylether
  5. filtrationcollected by filtration

출처 및 근거

ORD 기록
ord-f515df2394f34b938f3b61ccbfa8d63d
출처 데이터셋
uspto-grants-2000_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06156903

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