Potassium Carbonate → 1-(2-(5-Bromo-4-(5-chlorothiophen-2-yl)pyrimidin-2-ylamino)ethyl)imidazolidin-2-one

HRID 507671

Reaktionsgleichung

[Br:1][C:2]1[C:3]([C:9]2[S:10][C:11]([Cl:14])=[CH:12][CH:13]=2)=[N:4][C:5](Cl)=[N:6][CH:7]=1.C(=O)([O-])[O-].[K+].[K+].[NH2:21][CH2:22][CH2:23][N:24]1[CH2:28][CH2:27][NH:26][C:25]1=[O:29].C(=O)(O)[O-].[Na+]>CN1CCCC1=O>[Br:1][C:2]1[C:3]([C:9]2[S:10][C:11]([Cl:14])=[CH:12][CH:13]=2)=[N:4][C:5]([NH:21][CH2:22][CH2:23][N:24]2[CH2:28][CH2:27][NH:26][C:25]2=[O:29])=[N:6][CH:7]=1

Komponenten

Reaktionsbedingungen

Temperatur: 150 °C

Versuchsvorschrift

5-Bromo-2-chloro-4-(5-chlorothiophen-2-yl)pyrimidine (0.4g, 1.3 mmol), N-methyl pyrrolidone (3 mL), potassium carbonate (0.358 g, 2.6 mmol) and 1-(2-aminoethyl)-imidazolidin-2-one (0.2 g, 1.54 mmol) were all placed in a microwave tube. The reaction was heated to 150° C. for 20 min in a Personal Chemistry microwave. A saturated solution of sodium bicarbonate was added to the reaction mixtue, which was extracted three times with dichloromethane. The organic layer was dried with sodium sulfate and purified by flash chromatography on silica gel using gradient of 0 to 10% methanol in dichloromethane to obtain a white solid. Yield=0.41 g. MS (M+H)+ 402/404.

Aufarbeitung

customall placed in a microwave tube
extractionwas extracted three times with dichloromethane
dry with materialThe organic layer was dried with sodium sulfate
custompurified by flash chromatography on silica gel using gradient of 0 to 10% methanol in dichloromethane
customto obtain a white solid

Quellen und Nachweise

ORD-Eintrag: ord-9d2286de9ef54af1b45747777142b17a
Quelldatensatz: uspto-grants-2010_08
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US07786132B2

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