反应详情

A solution of 30 mg (0.16 mmol) 4-chloro-2-phenyl-pyrimidine (CAS: 14790-42-2), 42.8 mg (0.16 mmol) ((R)-3-Amino-pyrrolidin-1-yl)-(5-methyl-2-trifluoromethyl-phenyl)-methanone (intermediate 13), 54.3 mg (0.39 mmol) K2CO3 and 6.5 mg (0.039 mmol) KI in 1 mL N,N-dimethylacetamide was heated in a 60° C. for 2 h, and at 100° C. for 23 h. The solvent was removed in vacuo. The residue was dissolved in ethyl acetate and washed twice with water. The organic layer was dried with Na2SO4 and filtered. The mixture was concentrated and purified with flash column chromatography on silica eluting with a gradient formed from n-heptane and ethyl acetate to provide 31 mg (46%) of the titled compound as a light yellow solid. MS(m/e): 427.2 (M+H+).

1. customThe solvent was removed in vacuo
2. dissolutionThe residue was dissolved in ethyl acetate
3. washwashed twice with water
4. dry with materialThe organic layer was dried with Na2SO4
5. filtrationfiltered
6. concentrationThe mixture was concentrated
7. custompurified with flash column chromatography on silica eluting with a gradient
8. customformed from n-heptane and ethyl acetate