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Potassium Iodide → 8-(trifluoromethyl)-1-[(cyclopropylmethylamino)methyl]-6-(o-chlorophenyl)-4H-s-triazolo[4,3-a][1,4]benzodiazepine

HRID 596368
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 596368
[OH-].[K+].Cl.[CH:4]1([CH2:7][NH2:8])[CH2:6][CH2:5]1.[F:9][C:10]([F:35])([F:34])[C:11]1[CH:12]=[CH:13][C:14]2[N:20]3[C:21]([CH2:24]Cl)=[N:22][N:23]=[C:19]3[CH2:18][N:17]=[C:16]([C:26]3[CH:31]=[CH:30][CH:29]=[CH:28][C:27]=3[Cl:32])[C:15]=2[CH:33]=1.[I-].[K+]>CO.O1CCCC1>[F:35][C:10]([F:9])([F:34])[C:11]1[CH:12]=[CH:13][C:14]2[N:20]3[C:21]([CH2:24][NH:8][CH2:7][CH:4]4[CH2:6][CH2:5]4)=[N:22][N:23]=[C:19]3[CH2:18][N:17]=[C:16]([C:26]3[CH:31]=[CH:30][CH:29]=[CH:28][C:27]=3[Cl:32])[C:15]=2[CH:33]=1
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Komponenten

7

Edukt 4

HCID 4875Potassium IodideHCID 14797Potassium HydroxideHCID 81671(Cyclopropylmethyl)ammonium chlorideHCID 213307808-(trifluoromethyl)-1-(chloromethyl)-6-(o-chlorophenyl)-4H-s-triazolo[4,3-a][1,4]benzodiazepine

Produkt 1

HCID 214372888-(trifluoromethyl)-1-[(cyclopropylmethylamino)methyl]-6-(o-chlorophenyl)-4H-s-triazolo[4,3-a][1,4]benzodiazepine

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittelHCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

A stirred solution of potassium hydroxide (3.37 g., 0.06 mole) in methanol (30 ml.) is cooled in an ice bath, under nitrogen, and treated with (cyclopropylmethyl)-amine hydrochloride (6.45 g., 0.06 mole). The resulting mixture is kept in the ice bath for 15 minutes, treated with tetrahydrofuran (250 ml.), 8-(trifluoromethyl)-1-(chloromethyl)-6-(o-chlorophenyl)-4H-s-triazolo[4,3-a][1,4]benzodiazepine (6.86 g., 0.02 mole) and potassium iodide (3.32 g., 0.02 mole) and kept at ambient temperature for 18 hours. The mixture is concentrated and the residue is mixed with water and extracted with methylene chloride. The extract is washed with brine, dried over anhydrous sodium sulfate and concentrated. The product is crystallized once from ethyl acetate and once from methylene chloride ethyl acetate to give 8-(trifluoromethyl)-1-[[(cyclopropylmethyl)amino]methyl]-6-(o-chlorophenyl)-4H-s-triazolo[4,3-a][1,4]benzodiazepine. Preparation 28 8 -Chloro-1-[[(cyclopropylmethyl)amino] methyl]-6-(o-chlorophenyl)-4H-s-triazolo[4,3-a][1,4]benzodiazepine

Aufarbeitung

  1. concentrationThe mixture is concentrated
  2. additionthe residue is mixed with water
  3. extractionextracted with methylene chloride
  4. washThe extract is washed with brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. concentrationconcentrated
  7. customThe product is crystallized once from ethyl acetate and once from methylene chloride ethyl acetate

Quellen und Nachweise

ORD-Eintrag
ord-b85af1f64e684f52a0aff5d18ad57932
Quelldatensatz
uspto-grants-1977_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04010177

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