Triethylamine → HCID 59333671, Verbindung

1-Hydroxybenzotriazole monohydrate (38.2 mg, 0.25 mmol), 1-(dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (71.8 mg, 0.37 mmol), and triethylamine (52.2 μl, 0.37 mmol) were added to an N,N-dimethylformamide suspension (3.0 ml) of 5-[9-(cyclopropylmethyl)-6-morpholin-4-yl-8-piperazin-1-yl-9H-purin-2-yl]pyrimidin-2-amine (109.0 mg, 0.25 mmol) and imidazol-1-ylacetic acid (37.8 mg, 0.30 mmol) at room temperature. The resulting mixture was stirred for 17.5 hours and the reaction mixture was poured into dichloromethane-methanol (10:1), washed with saturated aqueous sodium hydrogen carbonate solution, and dried over anhydrous sodium sulfate. After filtration, the filtrate was concentrated under reduced pressure and the resulting residue was purified by preparative thin layer silica gel chromatography (dichloromethane:methanol=6:1) to give the title compound (108.0 mg, 79%) as a pale yellow solid.

1. washwashed with saturated aqueous sodium hydrogen carbonate solution
2. dry with materialdried over anhydrous sodium sulfate
3. filtrationAfter filtration
4. concentrationthe filtrate was concentrated under reduced pressure
5. customthe resulting residue was purified by preparative thin layer silica gel chromatography (dichloromethane:methanol=6:1)

ORD-Eintrag

ord-ab487bbefbbf46129a0e1afc8975ad43

Quelldatensatz

uspto-grants-2012_01

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08097622B2