反应详情

A mixture of Pd(dppf)Cl2.CH2Cl2 (65.3 mg, 0.08 mmol, 0.1 equiv.), N-tert-butyl-3-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)benzenesulfonamide (542 g, 1.60 mmol, 2.0 equiv.), 2-Bromo-N-(5-cyclopropyl-1H-pyrazol-3-yl)-5-((trimethyl silyl)ethynyl) pyrimidin-4-amine (300 mg, 0.80 mmol, 1.0 equiv.) and saturated aq Na2CO3 (10 mL) in dioxane (30 mL) was heated to 90° C. for 1 h under nitrogen atmosphere. The reaction mixture was cooled to room temperature and extracted with THF. The combined layers were concentrated and the residue was purified by silica gel chromatography (EtOAc/Petroleum ether from 10:1 to 1:1) to afford compound N-tert-butyl-3-(4-(3-cyclopropyl-1H-pyrazol-5-ylamino)-5-ethynylpyrimidin-2-yl)benzenesulfonamide (80 mg, 23%). LC-MS (m/z)=437.1 [M+H]+.

1. extractionextracted with THF
2. concentrationThe combined layers were concentrated
3. customthe residue was purified by silica gel chromatography (EtOAc/Petroleum ether from 10:1 to 1:1)