Potassium Iodide → 3-(3-(4-benzylpiperidin-1-yl)propyl)-6,7,8,9-tetrahydro-5H-1,2,4-triazolo[4,3-a]azepine

HRID 635272Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 635272
CS(Cl)(=O)=O.O[CH2:7][CH2:8][CH2:9][C:10]1[N:14]2[CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][C:13]2=[N:12][N:11]=1.[CH2:20]([CH:27]1[CH2:32][CH2:31][NH:30][CH2:29][CH2:28]1)[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1.C(=O)([O-])[O-].[K+].[K+].[I-].[K+]>CN(C)C=O.O.C(N(CC)CC)C>[CH2:20]([CH:27]1[CH2:32][CH2:31][N:30]([CH2:7][CH2:8][CH2:9][C:10]2[N:14]3[CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][C:13]3=[N:12][N:11]=2)[CH2:29][CH2:28]1)[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1

Komponenten

9

Edukt 5

HCID 4875Potassium IodideHCID 11430Potassium CarbonateHCID 31297Methanesulfonyl chlorideHCID 317384-BenzylpiperidineHCID 246884223-(3-hydroxypropyl)-6,7,8,9-tetrahydro-5H-1,2,4-triazolo[4,3-a]azepine

Produkt 1

HCID 155211573-(3-(4-benzylpiperidin-1-yl)propyl)-6,7,8,9-tetrahydro-5H-1,2,4-triazolo[4,3-a]azepine

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 962WaterLösungsmittelHCID 6228DimethylformamideLösungsmittelHCID 8471TriethylamineLösungsmittel

Versuchsvorschrift

Triethylamine (1.4 ml) and methanesulfonyl chloride (0.62 ml) were added to a solution of 3-(3-hydroxypropyl)-6,7,8,9-tetrahydro-5H-1,2,4-triazolo[4,3-a]azepine (0.98 g) obtained in the same manner as in Example 4 in dimethylformamide (20 ml) with stirring. Then, 4-benzylpiperidine (0.88 g), potassium carbonate (1.38 g) and potassium iodide (0.83 g) were added and the mixture was stirred for 4 hours at 60° C. After the completion of the reaction, the reaction mixture was poured into water, extracted with ethyl acetate, washed with water, and dried over magnesium sulfate. The solution was concentrated under reduced pressure to give 3-(3-(4-benzylpiperidin-1-yl)propyl)-6,7,8,9-tetrahydro-5H-1,2,4-triazolo[4,3-a]azepine.

Aufarbeitung

  1. stirringthe mixture was stirred for 4 hours at 60° C
  2. customAfter the completion of the reaction
  3. extractionextracted with ethyl acetate
  4. washwashed with water
  5. dry with materialdried over magnesium sulfate
  6. concentrationThe solution was concentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-bf5ce4330df84541bd33667931603c63
Quelldatensatz
uspto-grants-2001_02
Patentnummer
US06187774B1

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