反应详情

温度

110 °C

To a 35 ml seal tube, 1-(2-bromo-5-((2-(trimethylsilyl)ethoxy)methyl)-5H-pyrrolo[2,3-b]pyrazine-7-yl)-2,2-dimethylpropane-1-one (1.0 g, 0.00242 mole) and (6-aminopyridin-3-yl)methanol (0.36 g, 0.00291 mole) was taken in toluene (10.0 ml). The reaction mixture was purged with argon for 15 min at RT followed by Cs2CO3 (3.1 g, 0.0097 mole) was added and further purged for 30 min with argon. BINAP (0.03 g, 0.000048 mole) and Pd(OAc)2 (0.01 g, 0.000048 mole) were added and the reaction mixture was heated to 110° C. for 16 hrs. After completion of the reaction, the reaction mixture was filtered through celite bed and washed with ethyl acetate. Filtrate was collected and concentrated to afford crude product which was purified using column purification by eluting the compound with 20-25% ethyl acetate in hexanes to yield 0.5 g of 1-(2-(5-(hydroxymethyl)pyridin-2-ylamino)-5-((2-(trimethylsilyl)ethoxy)methyl)-5H-pyrrolo[2,3-b]pyrazin-7-yl)-2,2-dimethylpropan-1-one.

1. customTo a 35 ml seal tube
2. customThe reaction mixture was purged with argon for 15 min at RT
3. additionwas added
4. customfurther purged for 30 min with argon
5. customAfter completion of the reaction
6. filtrationthe reaction mixture was filtered through celite bed
7. washwashed with ethyl acetate
8. customFiltrate was collected
9. concentrationconcentrated
10. customto afford crude product which
11. customwas purified
12. customcolumn purification
13. washby eluting the compound with 20-25% ethyl acetate in hexanes