反应详情

A 1.0 M solution of ZnCl2 in Et2O (5.07 mL, 5.07 mmol) was added to a solution of 2,4-dichloro-5-(trifluoromethyl)pyrimidine (1.00 g, 4.61 mmol) in t-BuOH (25 mL) and DCE (25 mL) and the mixture was stirred for 10 minutes. The mixture was diluted with t-BuOH (25 mL) and DCE (25 mL) before 1-methyl-1H-pyrazol-4-amine (492 mg, 5.07 mmol) and Et3N (1.93 mL, 13.83 mmol) were added and stirring was continued at room temperature overnight. The volatiles were removed in vacuo and the resultant residue suspended in water (250 mL) and sonicated for 10 minutes. The solid was collected by vacuum filtration and the filter cake washed with water and then air dried. The solid was dissolved in DCM, adsorbed onto silica gel and purified by column chromatography (Biotage Isolera, 40 g SiO2 cartridge, 0-100% EtOAc in petroleum benzine 40-60° C.) to give the title compound A64 as a white solid (182 mg, 14%). LCMS-A: rt 6.113 min; m/z 278.1 [M+H]+.

1. additionwere added
2. stirringstirring
3. waitwas continued at room temperature overnight
4. customThe volatiles were removed in vacuo
5. customsonicated for 10 minutes
6. filtrationThe solid was collected by vacuum filtration
7. washthe filter cake washed with water
8. customair dried
9. dissolutionThe solid was dissolved in DCM
10. custompurified by column chromatography (Biotage Isolera, 40 g SiO2 cartridge, 0-100% EtOAc in petroleum benzine 40-60° C.)