Sodium Iodide → 1-[2-(2-Carboxy-4-chlorophenyl)amino-2-oxoethyl]-4-(2-oxo-1-benzimidazolinyl)piperidine

HRID 1899396

Reaktionsgleichung

Reaktionsgleichung von HRID 1899396
Cl[CH2:2][C:3]([NH:5][C:6]1[CH:11]=[CH:10][C:9]([Cl:12])=[CH:8][C:7]=1[C:13]([OH:15])=[O:14])=[O:4].[O:16]=[C:17]1[N:21]([CH:22]2[CH2:27][CH2:26][NH:25][CH2:24][CH2:23]2)[C:20]2[CH:28]=[CH:29][CH:30]=[CH:31][C:19]=2[NH:18]1.C(=O)([O-])[O-].[K+].[K+].[I-].[Na+]>CN(C=O)C.O>[C:13]([C:7]1[CH:8]=[C:9]([Cl:12])[CH:10]=[CH:11][C:6]=1[NH:5][C:3](=[O:4])[CH2:2][N:25]1[CH2:24][CH2:23][CH:22]([N:21]2[C:20]3[CH:28]=[CH:29][CH:30]=[CH:31][C:19]=3[NH:18][C:17]2=[O:16])[CH2:27][CH2:26]1)([OH:15])=[O:14]

Komponenten

7

Edukt 4

HCID 5238Sodium IodideHCID 11430Potassium CarbonateHCID 886381,3-Dihydro-1-(4-piperidinyl)-2H-benzimidazol-2-oneHCID 41798255-Chloro-2-((2-chloroacetyl)amino)benzoic acid

Produkt 1

HCID 152216631-[2-(2-Carboxy-4-chlorophenyl)amino-2-oxoethyl]-4-(2-oxo-1-benzimidazolinyl)piperidine

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

7.94 g (32 mmol) of the compound from Example II and 8.26 g (40 mmol) of 4-(2-oxo-1-benzimidazolinyl)piperidine (Aldrich) are initially introduced in 120 ml of DMF. The mixture is treated with 5.52 g (40 mmol) of potassium carbonate and 0.45 g (3 mmol) of sodium iodide and stirred overnight at room temperature. The batch is diluted with 600 ml of H2O and the product is precipitated at pH 5 by dropwise addition of 33 ml of 1N hydrochloric acid. The precipitate is filtered off with suction, stirred with 300 ml of diethyl ether and dried in a high vacuum.

Aufarbeitung

  1. customthe product is precipitated at pH 5 by dropwise addition of 33 ml of 1N hydrochloric acid
  2. filtrationThe precipitate is filtered off with suction
  3. stirringstirred with 300 ml of diethyl ether
  4. customdried in a high vacuum

Quellen und Nachweise

ORD-Eintrag
ord-b10f7b49606e4a6586371f77f5c2fca8
Quelldatensatz
uspto-grants-1996_11
Patentnummer
US05571921

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