反应详情

温度

80 °C

A mixture of 1-(4-bromobenzoyl)-3-dimethylaminopyrrolidine (40 mg, 0.13 mmol), 4-amino-2,1,3-benzothiadiazole (23 mg, 0.13 mmol), potassium phosphate (27 mg, 0.13 mmol), tris(dibenzylideneacetone)dipalladium(0) (3 mg, 0.002 mmol), and CTC-Q-Phos (6 mg, 0.004 mmol) are heated to 80° C. for 16 h and concentrated in vacuo. The resultant residue is dissolved in a mixture of DMSO, methanol and water and purified by reverse-phase semi-preparative HPLC1 to give the title compound as a white powder (11 mg), identified by HPLC and mass spectral analyses. Retention Time, 1.74 min.; MS [368.6 m/e (M+H)]. 1Semi-preparative HPLC Conditions: A=0.02% TFA in water, B=0.02% TFA in acetonitrile, 10-95% B in 8 min., 34 mL/min, 50° C., 215 nm detection, Waters Xterra™ 20×50 mm column.

1. concentrationconcentrated in vacuo
2. dissolutionThe resultant residue is dissolved in a mixture of DMSO, methanol and water
3. custompurified by reverse-phase semi-preparative HPLC1