Dimethylformamide → HCID 68778503, Verbindung

HRID 2263057Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2263057
FC(F)(F)C(O)=O.[CH3:8][C:9]1[C:13]([CH3:14])=[C:12]([NH:15][C:16]([N:18]2[CH2:23][CH2:22][NH:21][CH2:20][CH2:19]2)=[O:17])[O:11][N:10]=1.Cl[C:25]1[S:29][N:28]=[C:27]([C:30]2[CH:35]=[CH:34][CH:33]=[C:32]([F:36])[CH:31]=2)[N:26]=1.C(N(CC)CC)C.CN(C)C=O>O>[CH3:8][C:9]1[C:13]([CH3:14])=[C:12]([NH:15][C:16]([N:18]2[CH2:19][CH2:20][N:21]([C:25]3[S:29][N:28]=[C:27]([C:30]4[CH:35]=[CH:34][CH:33]=[C:32]([F:36])[CH:31]=4)[N:26]=3)[CH2:22][CH2:23]2)=[O:17])[O:11][N:10]=1

Komponenten

6

Edukt 4

HCID 6228DimethylformamideHCID 8471TriethylamineHCID 463184475-Chloro-3-(3-fluorophenyl)-1,2,4-thiadiazoleHCID 68778028HCID 68778028, Verbindung

Produkt 1

HCID 68778503HCID 68778503, VerbindungAusbeute 44,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

A solution of N-(3,4-dimethylisoxazol-5-yl)piperazine-1-carboxamide trifluoroacetate (300 mg, 0.887 mmol), 5-chloro-3-(3-fluorophenyl)-1,2,4-thiadiazole (190 mg, 0.887 mmol), triethylamine (0.618 ml, 4.43 mmol) and N,N-dimethylformamide (3 ml) was stirred at room temperature for 2 hours and the reaction mixture was poured into water. A solid was collected by filtration and recrystallized from a mixed solvent of tetrahydrofuran and ethyl acetate to obtain the desired product (160 mg, 44.8%) as a solid.

Aufarbeitung

  1. filtrationA solid was collected by filtration
  2. customrecrystallized from a mixed solvent of tetrahydrofuran and ethyl acetate

Quellen und Nachweise

ORD-Eintrag
ord-1d139e1693df46fda1de5b45ec22a290
Quelldatensatz
uspto-grants-2010_12
Patentnummer
US07851473B2

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