Reaktionsgleichung
Cl[C:2]1[N:7]=[C:6]([NH2:8])[C:5]([C:9]2[NH:13][N:12]=[N:11][N:10]=2)=[CH:4][N:3]=1.CCN(C(C)C)C(C)C.[CH2:23]([NH2:30])[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1>O1CCOCC1>[CH2:23]([NH:30][C:2]1[N:7]=[C:6]([NH2:8])[C:5]([C:9]2[NH:13][N:12]=[N:11][N:10]=2)=[CH:4][N:3]=1)[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1Komponenten
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
In a microwave tube, 2-chloro-5-(1H-tetrazol-5-yl)pyrimidin-4-amine (200 mg, 1.0 mmol) was dissolved into 3 mL of dioxane and DIPEA (1.5 mmol, 1.5 eq.). After the addition of benzylamine (5.0 mmol, 5.0 eq.), the tube was capped and irradiated in a CEM Discover microwave reactor to 120° C. for a total of 60 minutes in three 20 minutes intervals. LC/MS was taken every 20 minutes to follow the disappearance of starting material. After the complete consumption of the starting material, the reaction was cooled to room temperature and a precipitate formed. This solid was collected by filtration, washed several times with water, then with hot EtOAc. It was dried under vacuum to afford 27 mg of desired product. This material was carried forward without further purification. MS (EI) for C12H12N8: 269 (M+H).
Aufarbeitung
- customthe tube was capped
- customirradiated in a CEM Discover microwave reactor to 120° C. for a total of 60 minutes in three 20 minutes intervals
- customAfter the complete consumption of the starting material
- customa precipitate formed
- filtrationThis solid was collected by filtration
- washwashed several times with water
- customIt was dried under vacuum
Quellen und Nachweise
- ORD-Eintrag
- ord-ae219e88bfab4212aac734d71344c1e0
- Quelldatensatz
- uspto-grants-2011_11
- Patentnummer
- US08053454B2
Verknüpfte Notizen
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