反应详情

A mixture of tert-butyl 2-(3-iodo-5-methyl-1H-pyrazolo[3,4-c]pyridin-1-yl)acetate (1.00 g, 2.55 mmol), Zn(CN)2 (329 mg, 2.55 mmol), Pd(dppf)Cl2 (208 mg, 0.25 mmol), Pd2(dba)3 (233 mg, 0.25 mmol), water (2.7 mL) and DMF (20 mL) was subjected to microwave irradiation at 120° C. for 30 min under argon. The reaction mixture was filtered through a pad of Celite and the filtrate was diluted with water and EtOAc. The phases were separated and the aqueous layer was extracted with EtOAc. The combined organic extracts were washed with brine, then dried (Phase separator) and concentrated under vacuum. The residual oil was purified by flash chromatography on silica gel (EtOAc/c-hexane 1:2 then 1:1). MS (LC/MS): 273.0 [M+H]+; tR (HPLC conditions k): 3.04 min.

1. customirradiation at 120° C. for 30 min under argon
2. filtrationThe reaction mixture was filtered through a pad of Celite
3. additionthe filtrate was diluted with water and EtOAc
4. customThe phases were separated
5. extractionthe aqueous layer was extracted with EtOAc
6. washThe combined organic extracts were washed with brine
7. customdried (Phase separator)
8. concentrationconcentrated under vacuum
9. customThe residual oil was purified by flash chromatography on silica gel (EtOAc/c-hexane 1:2
10. custom3.04 min.