N-(3-BROMO-4-FLUOROBENZOYL)MORPHOLINE

反应条件: temp:100.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A dimethylformamide solution (2 ml) of the obtained (3-bromo-4-fluoro-phenyl)-morpholin-4-yl-methanone crude product (56.1 mg), bis-(4-methoxy-benzyl)-[5-(2-morpholin-4-yl-6,7-dihydro-5H-pyrrolo[2,3-d]pyrimidin-4-yl)-pyrimidin-2-yl]-amine (70.0 mg, 0.130 mmol), palladium acetate (2.9 mg, 0.013 mmol), X-Phos (12.4 mg, 0.0261 mmol) and potassium phosphate (55.1 mg, 0.260 mmol) was degassed under ultrasonic irradiation, followed by stirring at 100° C. for 6 hours under a nitrogen atmosphere. The reaction mixture was cooled to room temperature, followed by dilution with dichloromethane (10 ml), which was washed with saturated aqueous sodium chloride solution (10 ml). The organic layer was dried over sodium sulfate, followed by concentration under reduced pressure, and the residue was purified by silica gel column chromatography (dichloromethane/methanol=50/1), to obtain [3-(4-{2-[bis-(4-methoxy-benzyl)-amino]-pyrimidin-5-yl}-2-morpholin-4-yl-5,6-dihydro-pyrrolo[2,3-d]pyrimidin-7-yl)-4-fluoro-phenyl]-morpholin-4-yl-methanone as a pale brown solid (90.0 mg, 93%). The reaction mixture was cooled to room temperature was washed with saturated aqueous sodium chloride solution (10 ml) The organic layer was dried over sodium sulfate followed by concentration under reduced pressure the residue was purified by silica gel column chromatography (dichloromethane/methanol=50/1)

反应条件: temp:100.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A dimethylformamide solution (2 ml) of the obtained (3-bromo-4-fluoro-phenyl)-morpholin-4-yl-methanone crude product (56.1 mg), bis-(4-methoxy-benzyl)-[5-(2-morpholin-4-yl-6,7-dihydro-5H-pyrrolo[2,3-d]pyrimidin-4-yl)-pyrimidin-2-yl]-amine (70.0 mg, 0.130 mmol), palladium acetate (2.9 mg, 0.013 mmol), X-Phos (12.4 mg, 0.0261 mmol) and potassium phosphate (55.1 mg, 0.260 mmol) was degassed under ultrasonic irradiation, followed by stirring at 100° C. for 6 hours under a nitrogen atmosphere. The reaction mixture was cooled to room temperature, followed by dilution with dichloromethane (10 ml), which was washed with saturated aqueous sodium chloride solution (10 ml). The organic layer was dried over sodium sulfate, followed by concentration under reduced pressure, and the residue was purified by silica gel column chromatography (dichloromethane/methanol=50/1), to obtain [3-(4-{2-[bis-(4-methoxy-benzyl)-amino]-pyrimidin-5-yl}-2-morpholin-4-yl-5,6-dihydro-pyrrolo[2,3-d]pyrimidin-7-yl)-4-fluoro-phenyl]-morpholin-4-yl-methanone as a pale brown solid (90.0 mg, 93%). The reaction mixture was cooled to room temperature was washed with saturated aqueous sodium chloride solution (10 ml) The organic layer was dried over sodium sulfate followed by concentration under reduced pressure the residue was purified by silica gel column chromatography (dichloromethane/methanol=50/1)

反应条件: temp:100.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A dimethylformamide solution (2 ml) of the obtained (3-bromo-4-fluoro-phenyl)-morpholin-4-yl-methanone crude product (56.1 mg), bis-(4-methoxy-benzyl)-[5-(2-morpholin-4-yl-6,7-dihydro-5H-pyrrolo[2,3-d]pyrimidin-4-yl)-pyrimidin-2-yl]-amine (70.0 mg, 0.130 mmol), palladium acetate (2.9 mg, 0.013 mmol), X-Phos (12.4 mg, 0.0261 mmol) and potassium phosphate (55.1 mg, 0.260 mmol) was degassed under ultrasonic irradiation, followed by stirring at 100° C. for 6 hours under a nitrogen atmosphere. The reaction mixture was cooled to room temperature, followed by dilution with dichloromethane (10 ml), which was washed with saturated aqueous sodium chloride solution (10 ml). The organic layer was dried over sodium sulfate, followed by concentration under reduced pressure, and the residue was purified by silica gel column chromatography (dichloromethane/methanol=50/1), to obtain [3-(4-{2-[bis-(4-methoxy-benzyl)-amino]-pyrimidin-5-yl}-2-morpholin-4-yl-5,6-dihydro-pyrrolo[2,3-d]pyrimidin-7-yl)-4-fluoro-phenyl]-morpholin-4-yl-methanone as a pale brown solid (90.0 mg, 93%). The reaction mixture was cooled to room temperature was washed with saturated aqueous sodium chloride solution (10 ml) The organic layer was dried over sodium sulfate followed by concentration under reduced pressure the residue was purified by silica gel column chromatography (dichloromethane/methanol=50/1)