N-methyl-2-pyrrolidone → 5-{8-[(3R)-3-Ethylpiperazin-1-yl]-6-morpholin-4-yl-9-(2,2,2-trifluoroethyl)-9H-purin-2-yl}pyrimidin-2-amine

온도

100 °C

Diisopropylethylamine (1.91 ml, 10.98 mmol) was added to an N-methyl-2-pyrrolidone suspension (5 ml) of 2-(R)-ethylpiperazine-2-hydrochloride (751 mg) and 2-(2-aminopyrimidin-5-yl)-8-chloro-6-(morpholin-4-yl)-9-(2,2,2-trifluoroethyl)-9H-purine (506 mg, 1.22 mmol) and the resulting mixture was heated at 100° C. and stirred for 5 days. Water was added to the reaction mixture and the resulting mixture was extracted twice with ethyl acetate. The organic layers were combined, washed with water and saturated brine, and dried over anhydrous sodium sulfate, the mixture was filtrated, the filtrate was concentrated under reduced pressure, and the resulting residue was purified by silica gel chromatography (chloroform:methanol=97:3 to 90:10) to give the title compound (562 mg) as a pale yellow solid.

1. extractionthe resulting mixture was extracted twice with ethyl acetate
2. washwashed with water and saturated brine
3. dry with materialdried over anhydrous sodium sulfate
4. filtrationthe mixture was filtrated
5. concentrationthe filtrate was concentrated under reduced pressure
6. customthe resulting residue was purified by silica gel chromatography (chloroform:methanol=97:3 to 90:10)

ORD 기록

ord-92c992c3acef4af3b0950e8838115884

출처 데이터셋

uspto-grants-2012_01

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US08097622B2