Water → HCID 68782168, Verbindung

HRID 2262884

Reaktionsgleichung

Reaktionsgleichung von HRID 2262884
Cl[C:2]1[S:6][N:5]=[C:4]([CH:7]([CH3:9])[CH3:8])[N:3]=1.FC(F)(F)C(O)=O.[O:17]1[C:21]2[CH:22]=[CH:23][CH:24]=[CH:25][C:20]=2[C:19]([NH:26][C:27]([N:29]2[CH2:34][CH2:33][NH:32][CH2:31][CH2:30]2)=[O:28])=[N:18]1.C(N(CC)CC)C.O>CN(C)C=O>[O:17]1[C:21]2[CH:22]=[CH:23][CH:24]=[CH:25][C:20]=2[C:19]([NH:26][C:27]([N:29]2[CH2:34][CH2:33][N:32]([C:2]3[S:6][N:5]=[C:4]([CH:7]([CH3:9])[CH3:8])[N:3]=3)[CH2:31][CH2:30]2)=[O:28])=[N:18]1

Komponenten

6

Edukt 4

HCID 962WaterHCID 8471TriethylamineHCID 128746835-Chloro-3-(propan-2-yl)-1,2,4-thiadiazoleHCID 68778018HCID 68778018, Verbindung

Produkt 1

HCID 68782168HCID 68782168, VerbindungAusbeute 20,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

To a solution of 5-chloro-3-isopropyl-1,2,4-thiadiazole (90.3 mg, 0.555 mmol) and N-1,2-benzisoxazol-3-ylpiperazine-1-carboxamide trifluoroacetate (200 mg, 0.555 mmol) in N,N-dimethylformamide (2 ml) was added triethylamine (0.389 ml, 2.78 mmol) at room temperature, and the mixture was stirred at room temperature for 2 hours. The reaction mixture was poured to water, and the precipitated solid was separated by filtration, which was recrystallized from a mixed solvent of ethyl acetate and tetrahydrofuran to give 42.0 mg (20.3%) of the desired product. mp 178-179° C.

Aufarbeitung

  1. customthe precipitated solid was separated by filtration, which
  2. customwas recrystallized from a mixed solvent of ethyl acetate and tetrahydrofuran

Quellen und Nachweise

ORD-Eintrag
ord-55e6b39fa5f7449ab40a57f5ce0dedc2
Quelldatensatz
uspto-grants-2010_12
Patentnummer
US07851473B2

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