3-(Dimethylamino)pyrrolidine → HCID 59333673, Verbindung
Reaktionsgleichung
Cl[C:2]1[N:3]([CH2:25][CH:26]2[CH2:28][CH2:27]2)[C:4]2[C:9]([N:10]=1)=[C:8]([N:11]1[CH2:16][CH2:15][O:14][CH2:13][CH2:12]1)[N:7]=[C:6]([C:17]1[C:18]([CH3:24])=[N:19][C:20]([NH2:23])=[N:21][CH:22]=1)[N:5]=2.[CH3:29][N:30]([CH3:36])[CH:31]1[CH2:35][CH2:34][NH:33][CH2:32]1>CN1CCCC1=O>[CH:26]1([CH2:25][N:3]2[C:2]([N:33]3[CH2:34][CH2:35][CH:31]([N:30]([CH3:36])[CH3:29])[CH2:32]3)=[N:10][C:9]3[C:4]2=[N:5][C:6]([C:17]2[C:18]([CH3:24])=[N:19][C:20]([NH2:23])=[N:21][CH:22]=2)=[N:7][C:8]=3[N:11]2[CH2:16][CH2:15][O:14][CH2:13][CH2:12]2)[CH2:28][CH2:27]1Komponenten
4
Reaktionsbedingungen
- Temperatur
- 120 °C
Versuchsvorschrift
N-Methylpyrrolidone (1 ml) was added to 5-[8-chloro-9-(cyclopropylmethyl)-6-morpholin-4-yl-9H-purin-2-yl]-4-methylpyrimidin-2-amine (100 mg, 0.25 mmol) and 3-(dimethylamino)pyrolidine (285 mg, 2.49 mmol) and the resulting mixture was stirred at 120° C. for 3.5 hours. The reaction mixture was partitioned with chloroform and saturated brine and the organic layer was washed with saturated brine and dried over magnesium sulfate. The solvent was concentrated under reduced pressure, then methylene chloride-ether was added to the residue, and the precipitate was collected by filtration, washed with ether, and dried under reduced pressure to give the title compound (55 mg, 46%) as a pale orange solid.
Aufarbeitung
- customThe reaction mixture was partitioned with chloroform and saturated brine
- washthe organic layer was washed with saturated brine
- dry with materialdried over magnesium sulfate
- concentrationThe solvent was concentrated under reduced pressure
- additionmethylene chloride-ether was added to the residue
- filtrationthe precipitate was collected by filtration
- washwashed with ether
- customdried under reduced pressure
Quellen und Nachweise
- ORD-Eintrag
- ord-5e5902278c66408f81f866b935670eb0
- Quelldatensatz
- uspto-grants-2012_01
- Patentnummer
- US08097622B2
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