Potassium Carbonate → 5-[4-Chloro-6-(4-methyl-benzylamino)-[1,3,5]-triazin-2-ylamino]-3-methyl-imidazolidine-2,4-dione

HRID 76337

Reaktionsgleichung

Reaktionsgleichung von HRID 76337
Cl[C:2]1[N:7]=[C:6]([Cl:8])[N:5]=[C:4]([NH:9][CH:10]2[NH:14][C:13](=[O:15])[N:12]([CH3:16])[C:11]2=[O:17])[N:3]=1.C(=O)([O-])[O-].[K+].[K+].[CH3:24][C:25]1[CH:32]=[CH:31][C:28]([CH2:29][NH2:30])=[CH:27][CH:26]=1>CN(C)C=O.O.C(OCC)(=O)C>[Cl:8][C:6]1[N:7]=[C:2]([NH:30][CH2:29][C:28]2[CH:31]=[CH:32][C:25]([CH3:24])=[CH:26][CH:27]=2)[N:3]=[C:4]([NH:9][CH:10]2[NH:14][C:13](=[O:15])[N:12]([CH3:16])[C:11]2=[O:17])[N:5]=1

Komponenten

7

Edukt 3

HCID 11430Potassium CarbonateHCID 660354-MethylbenzylamineHCID 866980675-(4,6-Dichloro-[1,3,5]triazin-2-ylamino)-3-methyl-imidazolidine-2,4-dione

Produkt 1

HCID 866980665-[4-Chloro-6-(4-methyl-benzylamino)-[1,3,5]-triazin-2-ylamino]-3-methyl-imidazolidine-2,4-dione

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 962WaterLösungsmittelHCID 6228DimethylformamideLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

To a stirred suspension of 5-(4,6-dichloro-[1,3,5]triazin-2-ylamino)-3-methyl-imidazolidine-2,4-dione (Example 1.3, Part D) (200 mg, 0.72 mmol) and potassium carbonate (219 mg, 1.59 mmol) in dimethylformamide (5 mL) at room temperature was added 4-methyl-benzylamine (0.1 mL, 0.79 mmol). The reaction mixture was stirred at 35° for 24 h and then diluted with water and ethyl acetate. The ethyl acetate layer was separated, dried and evaporated to give the crude product which was used directly in the next step.

Aufarbeitung

  1. customThe ethyl acetate layer was separated
  2. customdried
  3. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-5ddbdf7a5b7e43f8b9d86a7bce001542
Quelldatensatz
uspto-grants-2014_09
Patentnummer
US08835629B2

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