反应详情

4-[5-(4-Iodo-3-methyl-phenylcarbamoyl)-pyridin-2-yl]-piperazine-1-carboxylic acid tert-butyl ester (35 mg, 0.07 mmol) was dissolved in 30% TFA in CH2Cl2 solution at room temperature. The mixture was stirred for 30 min and then partitioned between EtOAc and H2O. The water layer was made basic by the addition of Na2CO3. The organic layer was then collected washed with water dried over Na2SO4, filtered and evaporated. The residue was dissolved in CH2Cl2 and treated with 2,2-dimethysuccinic anhydride (13 mg, 0.10 mmol). After stirring at room temperature for 4 h the mixture was concentrated to a residue and washed with excess of hexanes to afford the product. HRMS m/z calcd for C23H27N4O4I [M+H]+: 551.1150. Found: 551.1152.

1. custompartitioned between EtOAc and H2O
2. additionThe water layer was made basic by the addition of Na2CO3
3. customThe organic layer was then collected
4. washwashed with water
5. dry with materialdried over Na2SO4
6. filtrationfiltered
7. customevaporated
8. dissolutionThe residue was dissolved in CH2Cl2
9. stirringAfter stirring at room temperature for 4 h the mixture
10. concentrationwas concentrated to a residue
11. washwashed with excess of hexanes
12. customto afford the product