Water → 1-Allyl-3-{2-chloro-4-fluoro-5-[(tetrahydro-3-oxo-1H,3H-[1,3,4]thiadiazolo[3,4-a]-pyridazine-1-ylidene)amino]phenyl}-5-methyl-s-triazine-2,4,6(1H,3H,5H)-trione

HRID 1489

Reaktionsgleichung

[Cl:1][C:2]1[CH:7]=[C:6]([F:8])[C:5]([N:9]=[C:10]2[N:14]3[CH2:15][CH2:16][CH2:17][CH2:18][N:13]3[C:12](=[O:19])[S:11]2)=[CH:4][C:3]=1[N:20]1[C:25](=[O:26])[NH:24][C:23](=[O:27])[N:22]([CH3:28])[C:21]1=[O:29].C(=O)([O-])[O-].[K+].[K+].[CH2:36](Br)[CH:37]=[CH2:38].O>CC(C)=O>[CH2:36]([N:24]1[C:23](=[O:27])[N:22]([CH3:28])[C:21](=[O:29])[N:20]([C:3]2[CH:4]=[C:5]([N:9]=[C:10]3[N:14]4[CH2:15][CH2:16][CH2:17][CH2:18][N:13]4[C:12](=[O:19])[S:11]3)[C:6]([F:8])=[CH:7][C:2]=2[Cl:1])[C:25]1=[O:26])[CH:37]=[CH2:38]

Komponenten

Reaktionsbedingungen

Temperatur: 40 °C

Versuchsvorschrift

A mixture of 1-{2-chloro-4-fluoro-5-[(tetrahydro-3-oxo-1H,3H-[1,3,4]thiadiazolo[3,4-a]pyridazin-1-ylidene)-amino]phenyl}-3-methyl-s-triazine-2,4,6(1H,3H,5H)-trione (1.00 g, 2.27 mmol), potassium carbonate (0.627 g, 4.54 mmol) and allyl bromide (0.329 g, 2.72 mmol) in acetone is stirred overnight at 40° C. and poured into water. The aqueous mixture is extracted with ethyl acetate. The organic extract is washed with water, dried over anhydrous magnesium sulfate, and concentrated in vacuo to give the title product as a white glass (0.8 g) which is identified by NMR spectral analyses.

Aufarbeitung

extractionThe aqueous mixture is extracted with ethyl acetate
extractionThe organic extract
washis washed with water
dry with materialdried over anhydrous magnesium sulfate
concentrationconcentrated in vacuo

Quellen und Nachweise

ORD-Eintrag: ord-a7e627b3bd4d476c9aa919241c2544ff
Quelldatensatz: uspto-grants-1998_03
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US05726126

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