反应详情

温度

160 °C

2-(4-Fluorophenyl)-1-(2-cyclopentylamino-4-pyrimidinyl)-5-(chloro)imidazo[4,5-b]pyridine (100 mg; 0.25 mmol), R-(+)-BINAP (10 mg; 0.016 mmol), Pd2(dba)3 (22 mg; 0.024 mmol) are suspended in xylene (16 ml), morpholine (0.43 ml; 4.9 mmol) is added, followed by NaOtBu (47 mg; 0.49 mmol) and heated to 160° C. for 10 min. under argon. The reaction mixture is poured on water (100 ml) containing HOAc (2 ml) and extracted with TBME three times. The combined organic phases are washed with 2N Na2CO3, dried over Na2SO4 and evaporated to dryness. Purification via SiO2 chromatography (TBME/hexane 7:3 to 10:0) and recrystallisation from TBME yields the title compound as colorless crystals (22 mg: 19%).

1. additionThe reaction mixture is poured on water (100 ml)
2. extractionextracted with TBME three times
3. washThe combined organic phases are washed with 2N Na2CO3
4. dry with materialdried over Na2SO4
5. customevaporated to dryness
6. customPurification
7. customvia SiO2 chromatography (TBME/hexane 7:3 to 10:0) and recrystallisation from TBME