反应详情

温度

85 °C

A mixture of 3-(4-iodopyrazol-1-yl)-propionic acid methyl ester (174 mg, 0.623 mmol), 3-benzothiazol-2-yl-5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-pyridin-2-ylamine (200.0 mg, 0.5662 mmol), Pd(PPh3)4 (50 mg, 0.04 mmol), potassium fluoride (98.7 mg, 1.70 mmol), and 4:1 dioxane:water (4:1, 1,4-dioxane:H2O, 8 mL) was heated in the microwave reactor at 85° C. for 30 min. The solution was concentrated in vacuo, and dry-loaded onto silica gel for column chromatography. The material was eluted with 2% MeOH/DCM. The fractions containing the product were concentrated in vacuo. The material was dissolved in conc. HCl (4 mL) and heated to 60° C. for 30 min in a sealed tube. The solvent was removed using the corrosive pump to afford the title compound as an orange solid. MS (ES+): m/z=366.14 (100) [MH+]. HPLC: tR=2.59 min (ZQ2, polar—5 min).

1. concentrationThe solution was concentrated in vacuo
2. washThe material was eluted with 2% MeOH/DCM
3. additionThe fractions containing the product
4. concentrationwere concentrated in vacuo
5. dissolutionThe material was dissolved in conc. HCl (4 mL)
6. temperatureheated to 60° C. for 30 min in a sealed tube
7. customThe solvent was removed