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Bromine → N-{5-[(2-amino[1,3]thiazolo[5,4-b]pyridin-5-yl)oxy]-2-chlorophenyl}-2,2,2-trifluoroacetamide

HRID 2366779
ノート
印刷プレビュー

反応式

HRID 2366779 の反応式
[NH2:1][C:2]1[CH:3]=[CH:4][C:5]([O:8][C:9]2[CH:10]=[CH:11][C:12]([Cl:22])=[C:13]([NH:15][C:16](=[O:21])[C:17]([F:20])([F:19])[F:18])[CH:14]=2)=[N:6][CH:7]=1.[S-:23][C:24]#[N:25].[K+].BrBr>C(O)(=O)C>[NH2:25][C:24]1[S:23][C:7]2[C:2]([N:1]=1)=[CH:3][CH:4]=[C:5]([O:8][C:9]1[CH:10]=[CH:11][C:12]([Cl:22])=[C:13]([NH:15][C:16](=[O:21])[C:17]([F:20])([F:18])[F:19])[CH:14]=1)[N:6]=2
参加物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 24408BromineHCID 516872Potassium thiocyanateHCID 57387327N-{5-[(5-aminopyridin-2-yl)oxy]-2-chlorophenyl}-2,2,2-trifluoroacetamide

生成物 1

HCID 57384282N-{5-[(2-amino[1,3]thiazolo[5,4-b]pyridin-5-yl)oxy]-2-chlorophenyl}-2,2,2-trifluoroacetamide収率 72%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

N-{5-[(5-Aminopyridin-2-yl)oxy]-2-chlorophenyl}-2,2,2-trifluoroacetamide (12 g, 36.2 mmol) and potassium thiocyanate (14.1 g, 145 mmol) were suspended in acetic acid (145 mL), bromine (8.67 g, 54.3 mmol) was added dropwise under ice-cooling, and the reaction mixture was stirred at room temperature for 16 hr. The reaction mixture was filtered through celite, and the filtrate was concentrated under reduced pressure. The residual oily substance was dissolved in ethyl acetate (100 mL), and aqueous sodium hydrogen carbonate solution (150 mL) was gradually added to partition the solution. The organic layer was dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residual solid was collected by filtration with diisopropyl ether (100 mL), and dried to give the title compound (10.1 g, 72%) as a pale-yellow solid.

後処理

  1. temperaturecooling
  2. filtrationThe reaction mixture was filtered through celite
  3. concentrationthe filtrate was concentrated under reduced pressure
  4. dissolutionThe residual oily substance was dissolved in ethyl acetate (100 mL)
  5. additionaqueous sodium hydrogen carbonate solution (150 mL) was gradually added
  6. customto partition the solution
  7. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  8. concentrationconcentrated under reduced pressure
  9. filtrationThe residual solid was collected by filtration with diisopropyl ether (100 mL)
  10. customdried

出典と根拠

ORDレコード
ord-e01ed5c33dde46fd8480aeefe5fef612
出典データセット
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08697874B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート