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

HRID 368455
ノート
印刷プレビュー

反応式

HRID 368455 の反応式
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]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

反応条件

温度
40 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-c6e8ca0371a344e8b40cc21463dd53a9
出典データセット
uspto-grants-2000_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06133284

反応ノート

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