Morpholine → Bis-(4-methoxy-benzyl)-{5-[2-morpholin-4-yl-7-(2-morpholin-4-yl-pyridin-4-yl)-6,7-dihydro-5H-pyrrolo[2,3-d]pyrimidin-4-yl]-pyrimidin-2-yl}-amine

温度

110 °C

To a solution of {5-[7-(2-chloro-pyridin-4-yl)-2-morpholin-4-yl-6,7-dihydro-5H-pyrrolo[2,3-d]pyrimidin-4-yl]-pyrimidin-2-yl}-bis-(4-methoxy-benzyl)-amine (50 mg) obtained in Step A, sodium t-butoxide (50 mg) and palladium dibenzylideneacetone complex (6 mg) suspended in toluene (1.5 ml), argon gas was blown for 5 minutes. Morpholine (10 μl) and 2,8,9-triisobutyl-2,5,8,9-tetraaza-1-phospha-bicyclo[3.3.3]undecane (6.9 mg) were added, followed by stirring at 110° C. for 6 hours. The reaction mixture was cooled to room temperature, and water (5 ml) was added, followed by extraction with dichloromethane (10 ml×2). The combined organic layers were washed with brine, and dried over sodium sulfate. After the drying agent was filtered off, the filtrate was concentrated under reduced pressure, and the resulting residue was purified by silica gel column chromatography (dichloromethane/methanol=50/1), to obtain a yellow amorphous (46 mg, 85%).

1. temperatureThe reaction mixture was cooled to room temperature
2. extractionfollowed by extraction with dichloromethane (10 ml×2)
3. washThe combined organic layers were washed with brine
4. dry with materialdried over sodium sulfate
5. filtrationAfter the drying agent was filtered off
6. concentrationthe filtrate was concentrated under reduced pressure
7. customthe resulting residue was purified by silica gel column chromatography (dichloromethane/methanol=50/1)
8. customto obtain a yellow amorphous (46 mg, 85%)

ORDレコード

ord-a35c989852c342918a269b4d1d428ef9

出典データセット

uspto-grants-2011_09

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08022205B2