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Potassium Iodide → 9-[4-chloro-3-(trifluoromethyl)benzyl]-4,9-dihydro-10H-thieno[3,4-b][1,5]benzodiazepin-10-one

HRID 1863188
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1863188
[CH:1]1[S:2][CH:3]=[C:4]2[C:10]=1[C:9](=[O:11])[NH:8][C:7]1[CH:12]=[CH:13][CH:14]=[CH:15][C:6]=1[NH:5]2.[H-].[Na+].[Cl:18][C:19]1[CH:26]=[CH:25][C:22]([CH2:23]Cl)=[CH:21][C:20]=1[C:27]([F:30])([F:29])[F:28].[I-].[K+]>CN(C)C=O>[Cl:18][C:19]1[CH:26]=[CH:25][C:22]([CH2:23][N:8]2[C:7]3[CH:12]=[CH:13][CH:14]=[CH:15][C:6]=3[NH:5][C:4]3=[CH:3][S:2][CH:1]=[C:10]3[C:9]2=[O:11])=[CH:21][C:20]=1[C:27]([F:28])([F:29])[F:30]
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Komponenten

6

Edukt 4

HCID 4875Potassium IodideHCID 24758Sodium hydrideHCID 125216414,9-dihydro-10H-thieno[3,4-b][1,5]benzodiazepin-10-oneHCID 130942621-Chloro-4-(chloromethyl)-2-(trifluoromethyl)benzene

Produkt 1

HCID 203922589-[4-chloro-3-(trifluoromethyl)benzyl]-4,9-dihydro-10H-thieno[3,4-b][1,5]benzodiazepin-10-one

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

To a solution of 8.64 g. of 4,9-dihydro-10H-thieno[3,4-b][1,5]benzodiazepin-10-one in 100 ml. of dimethylformamide is added 2.1 g. of 50% sodium hydride in mineral oil. The mixture is stirred for one hour and 10.0 g. of 4-chloro-3-trifluoromethyl benzyl chloride and 10 mg of potassium iodide are added. The mixture is stirred for a prolonged period and the solvent is removed in vacuo. The residual gum is dissolved in methylene chloride, dried over magnesium sulfate and filtered through magnesol. The filtrate is evaporated to give tan crystals which are recrystallized from ethanol giving the desired product as off-white crystals, mp. 181°-183° C.

Aufarbeitung

  1. stirringThe mixture is stirred for a prolonged period
  2. customthe solvent is removed in vacuo
  3. dissolutionThe residual gum is dissolved in methylene chloride
  4. dry with materialdried over magnesium sulfate
  5. filtrationfiltered through magnesol
  6. customThe filtrate is evaporated
  7. customto give tan crystals which
  8. customare recrystallized from ethanol giving the desired product as off-white crystals, mp. 181°-183° C.

Quellen und Nachweise

ORD-Eintrag
ord-4b9804bd98b641c691ff56b341ba740a
Quelldatensatz
uspto-grants-1979_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04168269

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